CN110357142B - Method and system for treating copper-containing etching waste liquid - Google Patents
Method and system for treating copper-containing etching waste liquid Download PDFInfo
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- CN110357142B CN110357142B CN201910688391.3A CN201910688391A CN110357142B CN 110357142 B CN110357142 B CN 110357142B CN 201910688391 A CN201910688391 A CN 201910688391A CN 110357142 B CN110357142 B CN 110357142B
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Abstract
The invention relates to the technical field of wastewater treatment, and provides a method and a system for treating copper-containing etching waste liquid. The method comprises the following steps: mixing the acidic etching waste liquid and the alkaline etching waste liquid to obtain a neutralized liquid; contacting the neutralized liquid with oxygen to obtain an oxidized liquid; carrying out pressure filtration on the oxidation liquid; pulping the first filter cake, and performing pressure filtration on the first slurry; pulping the second filter cake, and reacting the obtained second slurry with concentrated sulfuric acid; and (3) sequentially carrying out cooling crystallization and solid-liquid separation on the reaction liquid containing the copper sulfate to obtain copper sulfate crystals and copper sulfate mother liquor. According to the invention, the copper-containing acidic etching waste liquid is neutralized, then the neutralizing liquid is aerated, as the cuprous ions in the neutralizing liquid and the chloride ions form a complex, the cuprous ions are quickly oxidized into copper ions under the aeration state to form basic copper chloride precipitate, and then the basic copper chloride precipitate is recovered by filter pressing and is used for preparing copper sulfate, so that the copper concentration of the waste water is reduced, and the recovery rate of copper is improved.
Description
Technical Field
The invention relates to the technical field of printed circuit board wastewater treatment, in particular to a method and a system for treating copper-containing etching waste liquid.
Background
In the manufacturing process of the printed circuit board, the total copper content in the produced copper etching waste liquid is more than 6 million tons/month, the copper-containing etching waste liquid comprises acidic waste liquid and alkaline waste liquid, the main components of the acidic waste liquid are copper chloride and hydrochloric acid, the main components of the alkaline waste liquid are copper ammonia liquid and ammonia water, copper is a heavy metal element existing in soil and human and livestock bodies, the content of the copper in the soil is about 0.2ppm generally, excessive copper can generate precipitation/complexation reaction with enzymes in the human and livestock bodies, and the enzyme poisoning is generated to lose physiological functions. Therefore, a large amount of copper etching waste liquid generated in the manufacturing process of the printed circuit board will cause serious hidden danger of pollution to the environment, especially water resources and soil in the surrounding areas of the printed circuit board factory if not effectively treated in time.
In the prior art, the general treatment process of the copper-containing acidic etching waste liquid is a neutralization precipitation method, and the concentration of copper in the treated waste water is higher.
In view of the above, it is an urgent technical problem in the art to provide a new method for treating copper-containing etching waste liquid to overcome the above drawbacks in the prior art.
Disclosure of Invention
The present invention is directed to a method and a system for treating a copper-containing etching waste solution.
The object of the invention can be achieved by the following technical measures:
the invention provides a method for treating copper-containing etching waste liquid, which comprises the following steps:
s1, mixing the acidic etching waste liquid and the alkaline etching waste liquid to neutralize the acidic etching waste liquid to obtain a neutralized liquid;
s2, contacting the neutralized liquid with oxygen to oxidize cuprous ions in the neutralized liquid to obtain an oxidized liquid;
s3, performing pressure filtration on the oxidation solution to obtain a first waste liquid and a first filter cake;
s4, adding the first filter cake into water for pulping, and performing pressure filtration on the obtained first slurry to obtain a second waste liquid and a second filter cake;
s5, adding the second filter cake into water for pulping, and reacting the obtained second slurry with concentrated sulfuric acid to obtain reaction liquid containing copper sulfate;
s6, cooling and crystallizing the reaction solution containing copper sulfate and performing solid-liquid separation to obtain copper sulfate crystals and copper sulfate mother liquor.
Preferably, in step S1, the pH of the obtained neutralized liquid is 4-5.
Preferably, step S1 includes: in a neutralization reaction tank, mixing acidic etching waste liquid and alkaline etching waste liquid under stirring to neutralize the acidic etching waste liquid to obtain neutralized liquid;
the processing method further comprises the following steps: and refluxing the copper sulfate mother liquor to a neutralization tank.
Preferably, in step S2, the contacting the neutralizing liquid with oxygen includes:
introducing air or oxygen into the neutralizing liquid;
or, spraying the neutralization solution in air or oxygen;
or continuously updating the liquid level of the neutralizing liquid to promote the transfer of air or oxygen from the gas-liquid interface to the liquid phase.
Preferably, step S3 further includes: washing the obtained first filter cake; step S4 further includes: washing the second filter cake.
Preferably, step S3 includes:
introducing the oxidizing liquid into a filter press, and performing pressure filtration on the oxidizing liquid through pressure generated by a filter-pressing centrifugal pump of the filter press to form a first filter cake;
and introducing a washing liquid into a water pipe of the filter press, and enabling the washing liquid to flow through the first filter cake by using the pressure generated by a washing centrifugal pump of the filter press so as to wash the first filter cake.
Preferably, step S4 includes:
adding the first filter cake into water for pulping to obtain first slurry;
introducing the first slurry into a filter press, and performing pressure filtration on the first slurry by using pressure generated by a filter-pressing centrifugal pump of the filter press to form a second filter cake;
and introducing a washing liquid into a water pipe of the filter press, and enabling the washing liquid to flow through the second filter cake by using the pressure generated by a washing centrifugal pump of the filter press so as to wash the second filter cake.
Preferably, in step S5, the mass ratio of the copper content of the second slurry to the concentrated sulfuric acid is greater than or equal to 8: 11.
preferably, the density of the second slurry is 1.40kg/m3～1.50kg/m3。
In a second aspect, the present invention provides a copper-containing etching waste liquid treatment system, including: the system comprises a neutralization tank, an aeration device connected with the neutralization tank, a filter press connected with the aeration device, a pulping tank connected with the filter press, and an acidification crystallization reaction kettle connected with the pulping tank.
According to the method and the system for treating the copper-containing etching waste liquid, disclosed by the invention, after the copper-containing acidic etching waste liquid is neutralized, the neutralizing liquid is aerated, cuprous ions in the neutralizing liquid form a complex with chloride ions, the cuprous ions are quickly oxidized into copper ions under the aeration state to form basic copper chloride precipitate, and then the basic copper chloride precipitate is subjected to filter pressing recovery and is used for preparing copper sulfate, so that the copper recovery rate of copper is improved while the copper concentration of wastewater is reduced.
Drawings
FIG. 1 is a flow chart of a method for treating a copper-containing etching waste liquid according to an embodiment of the present invention.
FIG. 2 is a block diagram showing the structure of a copper-containing etching waste liquid treatment system according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to make the description of the present disclosure more complete and complete, the following description is given for illustrative purposes with respect to the embodiments and examples of the present invention; it is not intended to be the only form in which the embodiments of the invention may be practiced or utilized. The embodiments are intended to cover the features of the various embodiments as well as the method steps and sequences for constructing and operating the embodiments. However, other embodiments may be utilized to achieve the same or equivalent functions and step sequences.
The embodiment of the invention provides a method for treating copper-containing etching waste liquid, which is shown in figure 1 and comprises the following steps:
s1, mixing the acidic etching waste liquid and the alkaline etching waste liquid to neutralize the acidic etching waste liquid to obtain a neutralized liquid.
And S2, contacting the neutralized liquid with oxygen to oxidize cuprous ions in the neutralized liquid to obtain an oxidized liquid.
S3, performing pressure filtration on the oxidation liquid to obtain a first waste liquid and a first filter cake.
S4, adding the first filter cake into water for pulping, and performing pressure filtration on the obtained first slurry to obtain a second waste liquid and a second filter cake.
And S5, adding the second filter cake into water for pulping, and reacting the obtained second slurry with concentrated sulfuric acid to obtain reaction liquid containing copper sulfate.
S6, cooling and crystallizing the reaction solution containing copper sulfate and performing solid-liquid separation to obtain copper sulfate crystals and copper sulfate mother liquor.
An embodiment of the present invention further provides a system for treating copper-containing etching waste liquid, referring to fig. 2, where the system includes: a neutralization tank 10, an aeration device 20, a filter press 30, a beating tank 40 and an acidification crystallization reaction kettle 50.
The following describes the method for treating the copper-containing etching waste liquid in detail with reference to the copper-containing etching waste liquid treatment system.
First, in step S1, the acidic etching waste liquid and the alkaline etching waste liquid are respectively fed into the neutralization tank 10, and the acidic etching waste liquid and the alkaline etching waste liquid are mixed with stirring to perform a neutralization reaction, thereby obtaining a neutralized liquid.
In this embodiment, the acidic etching waste liquid includes cupric chloride, cuprous chloride, hydrochloric acid, and sodium chloride, wherein the copper content of the acidic etching waste liquid is 10% (mass%), and the acidic etching waste liquid includes 8.5% -9% (mass%) of copper ions and 1% -1.5% (mass%) of cuprous ions; the molar concentration of HCl in the acidic etching waste liquid is 1-2 mol/L, and the content of sodium chloride in the acidic etching waste liquid is 2-4% (mass percentage).
In this embodiment, the alkaline waste etching solution includes ammonium cupric chloride, ammonium hydroxide and ammonium chloride, wherein the ammonium cupric chloride and the ammonium hydroxide form a copper-ammonia complex, and the molecular formula of the copper-ammonia complex is Cu (NH)3)4Cl2The specific gravity of the copper-ammonia complex is about 1.18-1.25, and the copper content of the alkaline etching waste liquid is 10% (mass percentage); the molar concentration of ammonia water in the alkaline etching waste liquid is 7-9 mol/L.
Wherein, the pH value of the neutralizing solution is neutral, and cuprous ions and chloride ions form soluble complex under the neutral state. Further, the pH value of the neutralizing solution is controlled to be 4-5 by adjusting the volume ratio of the acidic etching waste solution and the alkaline etching waste solution which are introduced into the neutralizing tank 10.
Then, in step S2, the obtained neutralized liquid is introduced into the aeration device 20, and the neutralized liquid is contacted with oxygen to oxidize cuprous ions in the neutralized liquid, thereby obtaining an oxidized liquid.
In this embodiment, the manner of contacting the neutralizing liquid with oxygen may be one of the following: (1) introducing air or oxygen into the neutralizing liquid; or, (2) spraying the neutralization solution in air or oxygen; or (3) continuously updating the liquid level of the neutralizing liquid by adopting mechanical aeration to promote the air or oxygen to transfer from the gas-liquid interface to the liquid phase.
Specifically, the aeration apparatus 20 includes an aeration tank 201, an air diffusion unit 202 provided in the aeration tank 201, and an aeration pump 203 connected to the air diffusion unit 202 for supplying air or oxygen. The neutralized liquid is conveyed into the aeration tank 201, and is sufficiently contacted with air or oxygen emitted from the air diffusing unit 202, so that cuprous ions in the neutralized liquid are oxidized into copper ions, and the oxidized liquid is obtained.
Then, in step S3, the obtained oxidation liquid is sent to the filter press machine 30 to be subjected to pressure filtration, to obtain a first waste liquid and a first filter cake.
In this embodiment, the oxidizing liquid is introduced into the filter press 30, and the oxidizing liquid is pressure-filtered by the pressure generated by the filter-press centrifugal pump of the filter press 30 to form a first filter cake and a first waste liquid. Wherein the concentration of cuprous ions in the first waste liquid is 5-8 g/L. Further, the first filter cake is washed, a washing liquid is introduced into a water pipe of the filter press 30, and the washing liquid is caused to flow through the first filter cake by a pressure generated by a washing centrifugal pump of the filter press 30 to wash the first filter cake. And collecting a first washing liquid obtained after washing the first filter cake, combining the first washing liquid with the first waste liquid, wherein the concentration of cuprous ions in the combined waste liquid is 3-5 g/L.
Specifically, in the filter press 30, the pressure filtration is performed by the pressure of the filter press centrifugal pump, the filter cloth filters and retains the precipitate (forms a filter cake), and only the clear liquid can pass through the filter cloth (forms waste liquid), thereby achieving the effect of pressure filtration. In the washing step, a washing liquid (for example, water is used as the washing liquid) is introduced into a washing water pipe of the filter press, and water passes through the filter cake under the pressure of a washing centrifugal pump to dissolve and wash soluble salts in the filter cake. The operation adopts normal temperature operation, the filtration time is about 20 minutes, and the washing time is about 15 minutes.
Then, in step S4, the first filter cake is added to water to be beaten, and the resulting first slurry is subjected to pressure filtration to obtain a second waste liquid and a second filter cake.
In this embodiment, in the pulping tank 40, the first filter cake is added into water for pulping to obtain a first slurry; the first slurry is introduced into a filter press 30 and pressure filtered by pressure generated by a filter press centrifugal pump of the filter press 30 to form a second filter cake and a second waste stream. Wherein, the whole pulping process can be operated at normal temperature (for example, 5 ℃ to 35 ℃), and the pulping time can be 20 minutes to 40 minutes, for example, 30 minutes. Further, a washing liquid is introduced into the water pipe of the filter press machine 30, and the washing liquid is caused to flow through the second filter cake by the pressure generated by the washing centrifugal pump of the filter press machine 30 to wash the second filter cake. And collecting a second washing liquid obtained after washing the second filter cake, and combining the second washing liquid with the second waste liquid.
Specifically, the first filter cake of the first filter pressing enters the pulping tank 40, and is stirred and pulped with clean water (tap water) added in advance in the tank, the first filter cake is beaten into a slurry state again, soluble salt carried in the first filter cake can be dissolved in the pulping water, and the soluble salt is further removed through subsequent secondary filter pressing, so that the effect of more sufficient washing is achieved.
Combining the first washing liquid with the first waste liquid to obtain waste liquid, and further combining the second washing liquid with the second waste liquid to obtain waste liquid, wherein the final mixed wastewater (ammonia nitrogen wastewater) comprises the following components: about 140g/L of ammonium chloride, about 8-10 g/L of sodium chloride and 3-5 g/L of dissolved cuprous ions.
The total amount of the final mixed wastewater is about 6-7 tons of ammonia nitrogen wastewater per one ton of copper sulfate produced. As cuprous ions are soluble in the ammonium chloride wastewater and cannot be recycled through precipitation and filter pressing, resources are wasted, and the subsequent wastewater treatment pressure is increased, it should be understood by those skilled in the art that in other embodiments, the cuprous ions in the collected final mixed wastewater can be further oxidized into cupric ions, the copper content in the final wastewater is further reduced, and the cupric ions are further recycled.
Then, in step S5, the second filter cake is added to water for beating, and the obtained second slurry is reacted with concentrated sulfuric acid to obtain a reaction solution containing copper sulfate.
In this example, the second filter cake is added to water for pulping in a pulping tank 40 to obtain a second slurry. And (3) conveying the second slurry into an acidification crystallization reaction kettle 50, adding concentrated sulfuric acid into the acidification crystallization reaction kettle 50, dissolving the copper-containing precipitate in the second slurry into copper sulfate by sulfuric acid, and releasing heat to ensure that the temperature of the reaction solution reaches above 100 ℃. Further, the density of the second slurry obtained by beating is controlled to be 1.50kg/m3For example, 1.45kg/m3(ii) a The mass ratio of the copper content of the second slurry to the concentrated sulfuric acid is greater than or equal to 8: 11, for example, the concentrated sulfuric acid is added in an amount of about 550kg of concentrated sulfuric acid (excess sulfuric acid) per ton of copper sulfate, and is fed through a sulfuric acid metering tank. Further, the acidification crystallization reaction kettle 50 is an enamel reaction kettle. Further, the reaction time of the second slurry with concentrated sulfuric acid is less than or equal to 30 minutes.
Finally, in step S6, the reaction solution containing copper sulfate is sequentially cooled, crystallized and subjected to solid-liquid separation to obtain copper sulfate crystals and a copper sulfate mother liquor.
In this embodiment, crystallization is performed in the acidification crystallization reaction kettle 50, after the acidification reaction in the previous step is completed, the copper sulfate in the obtained reaction solution is nearly saturated, cooling water is introduced into a jacket of the acidification crystallization reaction kettle 50, the temperature of the copper sulfate solution is reduced from above 100 ℃ to 35-40 ℃ (the temperature in winter is lower, the temperature in summer is higher, and the temperature is higher), crystals of copper sulfate are precipitated, and a copper sulfate product is obtained through centrifugal separation/washing. The cooling crystallization time is 5-6 hours, and compared with winter, summer time is slightly longer. Further, the copper sulfate mother liquor may be refluxed into the neutralization tank 10.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A method for treating copper-containing etching waste liquid is characterized by comprising the following steps:
s1, mixing the acidic etching waste liquid and the alkaline etching waste liquid to neutralize the acidic etching waste liquid, and adjusting the volume ratio of the acidic etching waste liquid to the alkaline etching waste liquid to obtain a neutralized liquid; the pH value of the neutralization solution is 4-5; cuprous ions and chloride ions in the neutralization solution form soluble complexes;
s2, contacting the neutralized liquid with oxygen to oxidize cuprous ions in the neutralized liquid to obtain an oxidized liquid; the oxidizing solution comprises basic copper chloride precipitate obtained after the complex is oxidized;
s3, performing pressure filtration on the oxidation solution to obtain a first waste liquid and a first filter cake;
s4, adding the first filter cake into water for pulping, and performing pressure filtration on the obtained first slurry to obtain a second waste liquid and a second filter cake;
s5, adding the second filter cake into water for pulping, and reacting the obtained second slurry with concentrated sulfuric acid to obtain reaction liquid containing copper sulfate;
s6, cooling and crystallizing the reaction solution containing copper sulfate and performing solid-liquid separation to obtain copper sulfate crystals and copper sulfate mother liquor.
2. The method according to claim 1, wherein step S1 comprises: in a neutralization reaction tank, mixing acidic etching waste liquid and alkaline etching waste liquid under stirring to neutralize the acidic etching waste liquid to obtain neutralized liquid;
the processing method further comprises the following steps: and refluxing the copper sulfate mother liquor to a neutralization tank.
3. The method according to claim 1, wherein the contacting the neutralizing solution with oxygen in step S2 comprises:
introducing air or oxygen into the neutralizing liquid;
or, spraying the neutralization solution in air or oxygen;
or continuously updating the liquid level of the neutralizing liquid to promote the transfer of air or oxygen from the gas-liquid interface to the liquid phase.
4. The method according to claim 1, wherein the step S3 further comprises: washing the obtained first filter cake; step S4 further includes: washing the second filter cake.
5. The method according to claim 4, wherein the step S3 includes:
introducing the oxidizing liquid into a filter press, and performing pressure filtration on the oxidizing liquid through pressure generated by a filter-pressing centrifugal pump of the filter press to form a first filter cake;
and introducing a washing liquid into a water pipe of the filter press, and enabling the washing liquid to flow through the first filter cake by using the pressure generated by a washing centrifugal pump of the filter press so as to wash the first filter cake.
6. The method according to claim 4, wherein the step S4 includes:
adding the first filter cake into water for pulping to obtain first slurry;
introducing the first slurry into a filter press, and performing pressure filtration on the first slurry by using pressure generated by a filter-pressing centrifugal pump of the filter press to form a second filter cake;
and introducing a washing liquid into a water pipe of the filter press, and enabling the washing liquid to flow through the second filter cake by using the pressure generated by a washing centrifugal pump of the filter press so as to wash the second filter cake.
7. The method for treating etching waste liquid containing copper according to claim 1, wherein in step S5, the mass ratio of the copper content of the second slurry to the concentrated sulfuric acid is greater than or equal to 8: 11.
8. the method according to claim 1 or 7, wherein the second slurry has a density of between about 1.40kg/m and about 1.50kg/m for carrying out thin film etching.
9. A copper-containing etching waste liquid treatment system for use in the method for treating copper-containing etching waste liquid according to any one of claims 1 to 8, characterized in that the treatment system comprises: the system comprises a neutralization tank, an aeration device connected with the neutralization tank, a filter press connected with the aeration device, a pulping tank connected with the filter press, and an acidification crystallization reaction kettle connected with the pulping tank; the aeration device comprises an aeration tank, an air dispersion component arranged in the aeration tank and an aeration pump connected with the air dispersion component and used for conveying air or oxygen.
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| US20240343599A1 (en) * | 2021-12-31 | 2024-10-17 | Dongjiang Environmental Company Limited | Method for producing high purity copper sulfate from spent acidic copper chloride etching solution |
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