CN115928078A - Etching waste liquid cyclic regeneration and cuprous chloride, copper recovery system - Google Patents
Etching waste liquid cyclic regeneration and cuprous chloride, copper recovery system Download PDFInfo
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- CN115928078A CN115928078A CN202211591722.XA CN202211591722A CN115928078A CN 115928078 A CN115928078 A CN 115928078A CN 202211591722 A CN202211591722 A CN 202211591722A CN 115928078 A CN115928078 A CN 115928078A
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- 238000005530 etching Methods 0.000 title claims abstract description 349
- 239000007788 liquid Substances 0.000 title claims abstract description 267
- 239000010949 copper Substances 0.000 title claims abstract description 223
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 221
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 218
- 239000002699 waste material Substances 0.000 title claims abstract description 218
- 229910021591 Copper(I) chloride Inorganic materials 0.000 title claims abstract description 175
- 229940045803 cuprous chloride Drugs 0.000 title claims abstract description 175
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 title claims abstract description 169
- 238000011084 recovery Methods 0.000 title claims description 36
- 230000008929 regeneration Effects 0.000 title claims description 30
- 238000011069 regeneration method Methods 0.000 title claims description 30
- 125000004122 cyclic group Chemical group 0.000 title description 4
- 238000000605 extraction Methods 0.000 claims abstract description 169
- 238000004064 recycling Methods 0.000 claims abstract description 76
- 238000004519 manufacturing process Methods 0.000 claims abstract description 66
- 239000002253 acid Substances 0.000 claims abstract description 53
- 238000001914 filtration Methods 0.000 claims abstract description 39
- 230000002378 acidificating effect Effects 0.000 claims description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 56
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 47
- 238000005868 electrolysis reaction Methods 0.000 claims description 44
- 239000002244 precipitate Substances 0.000 claims description 44
- 239000000047 product Substances 0.000 claims description 18
- 238000000746 purification Methods 0.000 claims description 18
- 238000006386 neutralization reaction Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 13
- 230000000996 additive effect Effects 0.000 claims description 12
- 230000001172 regenerating effect Effects 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims 5
- BJBUTJQYZDYRMJ-UHFFFAOYSA-N Kaempferol 3,7-dimethyl ether Chemical compound C=1C(OC)=CC(O)=C(C(C=2OC)=O)C=1OC=2C1=CC=C(O)C=C1 BJBUTJQYZDYRMJ-UHFFFAOYSA-N 0.000 claims 2
- 230000003472 neutralizing effect Effects 0.000 abstract description 24
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000002585 base Substances 0.000 abstract 5
- 239000003513 alkali Substances 0.000 abstract 1
- 239000012043 crude product Substances 0.000 description 34
- 238000004140 cleaning Methods 0.000 description 19
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 7
- 229910001431 copper ion Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010668 complexation reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 239000003712 decolorant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- -1 mordants Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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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- ing And Chemical Polishing (AREA)
Abstract
The invention provides a system for recycling etching waste liquid and cuprous chloride and copper, wherein the system for recycling etching waste liquid comprises an acid-base etching waste liquid collecting and neutralizing device, a cuprous chloride filtering and recycling device and an acid-base etching liquid recycling device which are fixedly connected in sequence, the acid-base etching waste liquid collecting and neutralizing device is respectively connected with an etching waste liquid outlet of an acid etching production line, an etching waste liquid outlet of an alkaline etching production line and the cuprous chloride filtering and recycling device, the cuprous chloride filtering and recycling device is respectively connected with the acid-base etching liquid recycling device, the cuprous chloride purifying system and the electrolytic copper extraction recycling system, and the acid-base etching liquid recycling device is also respectively connected with the acid etching production line and the alkaline etching production line. The beneficial effects of the invention are as follows: different recycling systems of the acid and alkali etching waste liquid are integrated into a set of recycling system, the recycling quality of the etching waste liquid is high, the copper extraction efficiency is high, and the production cost of cuprous chloride is low.
Description
Technical Field
The invention relates to the field of etching waste liquid recycling, in particular to a system for recycling etching waste liquid and cuprous chloride and copper.
Background
At present, in a circuit board etching production line, a printed circuit board etching waste liquid recycling system is widely used. The etching of the printed circuit board is divided into two categories of acid etching and alkaline etching, and the cyclic regeneration treatment is basically carried out separately aiming at the cyclic regeneration of the etching waste liquid. The etching solution mainly comprises cuprous chloride, the cuprous chloride is widely applied to catalysts, bactericides, mordants, decolorants and metallurgical industry, the existing cuprous chloride production process is generated by the reaction of the cupric chloride and copper powder, and the manufacturing cost is high. The copper extraction mode is divided into alkaline extraction electrolysis copper extraction and direct electrolysis copper extraction in an alkaline recycling system, and the acidic membrane electrolysis copper extraction is also carried out in an acidic recycling system, so that a plurality of etching waste liquid recycling systems are required.
And because of the characteristics of the electrolytic copper extraction process, the practical production of the cuprous chloride crude product and the etching waste liquid recycling system has the following defects:
1. different recycling equipment is required to be arranged aiming at different systems, so that the equipment cost is high, and the matched floor area is large;
2. the existing copper extraction process can only reduce the concentration of copper ions in a regeneration sub-solution from 100g per liter to 30g-50g, the copper extraction efficiency is not high, and the efficiency of different copper recovery systems is different;
3. in the prior art, etching waste liquid needs to enter a copper extraction device, a small amount of additive needs to be added, impurities can be brought into the etching liquid, and the quality of the regenerated etching liquid is influenced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a system for recycling etching waste liquid and recovering cuprous chloride and copper, wherein the system for recycling etching waste liquid, the system for purifying cuprous chloride and the system for recovering electrolytic copper extraction are arranged in the system for recycling etching waste liquid, the crude cuprous chloride precipitate can be precipitated through the neutralization of acidic etching waste liquid and alkaline etching waste liquid, no additive is needed to be added, the etching waste liquid does not enter copper extraction equipment and can not bring impurities, the etching waste liquid is easy to recycle, the quality of the regenerated acid-base etching liquid is obviously improved, the consumption is only 1/5 of that of the regenerated acid-base etching liquid in the prior art, the cost of production materials is effectively reduced, different recycling systems of the acid-base etching waste liquid are integrated into a set of recycling systems, the occupied area of the equipment is small, and the equipment cost is low; the crude cuprous chloride precipitate can be purified and processed into a cuprous chloride finished product, the purity is up to more than 99%, the purification process only has a small amount of volatile matters of hydrochloric acid and ethanol, the tail gas treatment cost is low, and the production cost is reduced; the crude cuprous chloride precipitate can also be dissolved for electrolytic copper extraction, the copper ions in the etching waste liquid can be treated from 100g per liter to 5g-10g per liter, the extraction efficiency of copper is greatly improved, and the problems that in the current etching production line, the etching waste liquid needs to be provided with different recycling regeneration equipment, the current copper extraction process efficiency is not high, the etching liquid quality of the current etching waste liquid recycling regeneration system is low, and the current cuprous chloride production cost is high are solved.
The invention provides a system for recycling etching waste liquid and recovering cuprous chloride and copper, which comprises a system for recycling etching waste liquid, a system for purifying cuprous chloride and a system for recovering electrolytic copper, the etching waste liquid recycling system comprises an acid-base etching waste liquid collecting and neutralizing device, a cuprous chloride filtering and recovering device and an acid-base etching liquid regenerating device which are fixedly connected in sequence, the acid-base etching waste liquid collecting and neutralizing device is provided with an acid-base etching waste liquid inlet and a neutralized etching waste liquid outlet, the acid-base etching waste liquid water inlet is respectively connected with an etching waste liquid outlet of an acid etching production line and an etching waste liquid outlet of an alkaline etching production line, the neutralized etching waste liquid outlet is connected with the cuprous chloride filtering and recovering device, the cuprous chloride filtering and recovering device is provided with a filtered etching waste liquid outlet and a cuprous chloride precipitate outlet, the filtered waste etching liquid outlet is connected with the acid-base etching liquid regeneration device, the acid-base etching liquid regeneration device is also respectively connected with the acid etching production line and the alkaline etching production line, the cuprous chloride precipitate discharge port is respectively connected with the cuprous chloride purification system and the electrolytic copper extraction recovery system, a PH value detection sensor is also arranged in the acid-base etching waste liquid collecting and neutralizing device, the cuprous chloride filtering and recycling device can separate the etching waste liquid neutralized in the acid-base etching waste liquid collecting and neutralizing device from cuprous chloride precipitate, and the neutralized etching waste liquid is treated and adjusted into new acid-base etching liquid by the acid-base etching liquid regeneration device and is provided for etching production of an etching production line, the cuprous chloride precipitate is purified and recovered into a cuprous chloride finished product by a cuprous chloride purification system, and the cuprous chloride precipitate is recovered into a copper finished product by an electrolysis copper extraction recovery system.
The acid-base etching waste liquid collecting and neutralizing device comprises an alkaline etching waste liquid collecting tank, an acidic etching waste liquid collecting tank and an acid-base etching waste liquid neutralizing tank, wherein the acid-base etching waste liquid neutralizing tank is respectively communicated with the alkaline etching waste liquid collecting tank and the acidic etching waste liquid collecting tank, a neutralizing etching waste liquid outlet is fixedly arranged on the acid-base etching waste liquid neutralizing tank, the acid-base etching waste liquid water inlet comprises an acidic etching waste liquid water inlet and an alkaline etching waste liquid water inlet, the alkaline etching waste liquid collecting tank is communicated with an etching waste liquid outlet of an alkaline etching production line through the alkaline etching waste liquid water inlet, and the acidic etching waste liquid collecting tank is communicated with the etching waste liquid outlet of the acidic etching production line through the acidic etching waste liquid water inlet.
The cuprous chloride filtering and recycling device is further improved, the cuprous chloride filtering tank is arranged on the bottom side face of the cuprous chloride filtering tank, the filtered etching waste liquid outlet is formed in the bottom of the cuprous chloride filtering tank, the cuprous chloride precipitate outlet is formed in the bottom of the cuprous chloride filtering tank, and the neutralized etching waste liquid outlet is communicated with the cuprous chloride filtering tank.
The acid-base etching solution regeneration device is further improved and comprises a regeneration solution collection tank, an acid etching solution regenerator, an alkaline etching solution regenerator, an acid etching solution tank and an alkaline etching solution tank which are fixedly connected in sequence, wherein the regeneration solution collection tank is communicated with the filtered etching waste solution drainage port, the regeneration solution collection tank is respectively communicated with the acid etching solution regenerator and the alkaline etching solution regenerator, the acid etching solution regenerator is communicated with the acid etching solution tank, the alkaline etching solution regenerator is communicated with the alkaline etching solution tank, the acid etching solution tank is communicated with the acid etching production line, and the alkaline etching solution tank is communicated with the alkaline etching production line.
The invention is further improved, the additive added to the etching waste liquid in the acidic etching liquid regenerator is hydrochloric acid, and the additive added to the etching waste liquid in the alkaline etching liquid regenerator is ammonia water.
The invention is further improved, the cuprous chloride purification system comprises a dilute hydrochloric acid cleaning tank, a dilute hydrochloric acid filtering tank, an ethanol cleaning tank and an ethanol filtering tank which are fixedly connected in sequence, the cuprous chloride precipitate outlet is communicated with the dilute hydrochloric acid cleaning tank, the dilute hydrochloric acid filtering tank is provided with a cuprous chloride hydrochloric acid cleaning outlet and a dilute hydrochloric acid filtering liquid outlet, the cuprous chloride hydrochloric acid cleaning outlet is communicated with the ethanol cleaning tank, the dilute hydrochloric acid filtering liquid outlet is communicated with the dilute hydrochloric acid cleaning tank, the ethanol filtering tank is provided with a cuprous chloride finished product outlet and an ethanol filtering liquid outlet, and the ethanol filtering liquid outlet is communicated with the ethanol cleaning tank.
The invention is further improved, the electrolytic copper extraction recovery system is an extraction electrolytic copper extraction system, and comprises a cuprous chloride crude product extraction dissolving tank, an alkaline extraction high copper solution collecting tank, an alkaline extraction low copper solution collecting tank and an extraction copper extraction device, wherein the cuprous chloride crude product extraction dissolving tank is respectively communicated with the cuprous chloride precipitate discharge port and the alkaline extraction high copper solution collecting tank, the alkaline extraction high copper solution collecting tank is communicated with the extraction copper extraction device, the extraction copper extraction device is communicated with the alkaline extraction low copper solution collecting tank, and the alkaline extraction low copper solution collecting tank is communicated with the cuprous chloride crude product extraction dissolving tank.
The invention is further improved, the copper extraction device comprises an extraction tank, a rinsing tank, a back extraction tank and a copper recovery electrolytic tank, wherein the extraction tank is respectively communicated with the alkaline extraction high copper solution collection tank and the alkaline extraction low copper solution collection tank, the extraction tank, the rinsing tank, the back extraction tank and the copper recovery electrolytic tank are sequentially and fixedly connected, the alkaline high copper solution in the alkaline extraction high copper solution collection tank can be extracted in the extraction tank, and the extracted copper solution can flow into the back extraction tank to wash off residual alkaline high copper solution and then flow into the back extraction tank to perform back extraction, and then flow into the copper recovery electrolytic tank to perform electrolytic copper extraction.
The invention is further improved, the electrolytic copper-extracting recovery system is an alkaline direct electrolytic copper-extracting system, and comprises a cuprous chloride crude product alkaline dissolving tank, an alkaline electrolytic copper-extracting high copper solution collecting tank, an alkaline electrolytic copper-extracting low copper solution collecting tank and an alkaline direct electrolytic copper-extracting solution tank, wherein the cuprous chloride crude product alkaline dissolving tank, the alkaline electrolytic copper-extracting high copper solution collecting tank, the alkaline electrolytic copper-extracting low copper solution collecting tank and the alkaline direct electrolytic copper-extracting solution tank are fixedly communicated in sequence, and the alkaline direct electrolytic copper-extracting solution tank is also communicated with the cuprous chloride crude product alkaline dissolving tank.
The invention is further improved, the electrolytic copper extraction recovery system is an acidic direct-film electrolytic copper extraction system, and comprises a cuprous chloride crude product acidic dissolving tank, an acidic electrolytic copper extraction high copper solution collecting tank, an acidic electrolytic copper extraction low copper solution collecting tank and an acidic direct-film electrolytic copper extraction solution tank, wherein the cuprous chloride crude product acidic dissolving tank, the acidic electrolytic copper extraction high copper solution collecting tank, the acidic electrolytic copper extraction low copper solution collecting tank and the acidic direct-film electrolytic copper extraction solution tank are fixedly communicated in sequence, and the acidic direct electrolytic copper extraction solution tank is also communicated with the cuprous chloride crude product acidic dissolving tank and the acidic etching production line.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a system for recycling etching waste liquid, cuprous chloride and copper, which is characterized in that a system for recycling the etching waste liquid, a cuprous chloride purification system and an electrolytic copper extraction recovery system which are matched with each other are arranged in the system for recycling the etching waste liquid, a cuprous chloride filtering recovery device can separate the etching waste liquid from cuprous chloride precipitate after acid-base etching waste liquid is collected and neutralized in the neutralization device, the neutralized etching waste liquid is treated and adjusted into new acid-base etching liquid by the acid-base etching liquid regeneration device to be supplied to an etching production line for etching production, the cuprous chloride precipitate is purified and recovered into cuprous chloride finished products by the cuprous chloride purification system, the cuprous chloride precipitate is recovered into copper finished products by the electrolytic copper extraction recovery system, the cuprous chloride precipitate crude products can be precipitated by neutralizing the acid etching waste liquid and the alkaline etching waste liquid, no additive needs to be added, the etching waste liquid does not enter a copper extraction device, impurities can not be generated, the etching waste liquid is easy to be recycled, the quality of the regenerated etching waste liquid is obviously improved, only 1/5 of the acid-base etching liquid after the acid-base etching liquid is regenerated by the existing process, the production material is effectively reduced, the cost, a set of different recycling systems for recycling the acid-base etching waste liquid is integrated into a small system, and the regeneration system, and the area is integrated; the cuprous chloride precipitate crude product can be purified and processed into a cuprous chloride finished product, the purity is up to more than 99%, the purification process only has a small amount of volatile matters of hydrochloric acid and ethanol, the tail gas treatment cost is low, and the production cost is reduced; the cuprous chloride precipitate crude product can also be dissolved for electrolytic copper extraction, copper ions in the etching waste liquid can be treated from 100g per liter to 5g-10g per liter, the extraction efficiency of copper is greatly improved, and the problems that in the existing etching production line, different recycling and regenerating devices need to be arranged on the etching waste liquid, the existing copper extraction process efficiency is not high, the quality of the etching liquid of the existing etching waste liquid recycling and regenerating system is low, and the existing cuprous chloride production cost is high are solved.
Drawings
FIG. 1 is a schematic diagram of a system for recycling etching waste liquid and recovering cuprous chloride and copper according to the present invention;
FIG. 2 is a schematic diagram of a cuprous chloride purification system of the present invention;
FIG. 3 is a schematic diagram of the copper extraction system of the present invention;
FIG. 4 is a schematic diagram of an alkaline direct electrolytic copper extraction system according to the present invention;
FIG. 5 is a schematic diagram of an acidic direct film electrolytic copper extraction system according to the present invention;
FIG. 6 is a table showing the contents of copper ions before and after filtration in the system for recycling etching waste liquid according to the present invention.
In the figure, the position of the upper end of the main shaft, 1-etching waste liquid recycling and regenerating system, 11-acid-base etching waste liquid collecting and neutralizing device, 111-alkaline etching waste liquid collecting tank, 112-acid etching waste liquid collecting tank, 113-acid-base etching waste liquid neutralizing tank, 12-cuprous chloride filtering and recovering device, 121-cuprous chloride filter tank, 13-acid-base etching liquid regenerating device, 131-regenerating liquid collecting tank, 132-acid etching liquid regenerator, 133-alkaline etching liquid regenerator, 134-acid etching liquid tank, 135-alkaline etching liquid tank, 14-acid etching production line, 15-alkaline etching production line, 2-cuprous chloride purifying system, 21-dilute hydrochloric acid cleaning tank, 22-dilute hydrochloric acid filter tank, 23-ethanol cleaning tank, 24-ethanol filter tank, 3-electrolytic copper extraction and recovering system 4-extraction electrolysis copper extraction system, 41-cuprous chloride crude product extraction dissolving tank, 42-alkaline extraction high copper solution collecting tank, 43-alkaline extraction low copper solution collecting tank, 44-extraction copper extraction device, 441-extraction tank, 442-rinsing tank, 443-stripping tank, 444-copper recovery electrolytic tank, 5-alkaline direct electrolysis copper extraction system, 51-cuprous chloride crude product alkaline dissolving tank, 52-alkaline electrolysis copper extraction high copper solution collecting tank, 53-alkaline electrolysis copper extraction low copper solution collecting tank, 54-alkaline direct electrolysis copper extraction solution tank, 6-acidic direct membrane electrolysis copper extraction system, 61-cuprous chloride crude product acidic dissolving tank, 62-acidic electrolysis copper extraction high copper solution collecting tank, 63-acidic electrolysis copper extraction low copper solution collecting tank, 64-acid direct membrane electrolysis copper extraction solution tank.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
As shown in fig. 1-6, the etching waste liquid recycling system and cuprous chloride and copper recovery system provided by the invention comprises an etching waste liquid recycling system 1, a cuprous chloride purification system 2 and an electrolytic copper extraction recovery system 3, wherein the etching waste liquid recycling system 1 comprises an acid-base etching waste liquid collecting and neutralizing device 11, a cuprous chloride filtering and recovering device 12 and an acid-base etching liquid regenerating device 13 which are fixedly connected in sequence, the acid-base etching waste liquid collecting and neutralizing device 11 is provided with an acid-base etching waste liquid inlet and a neutralized etching waste liquid outlet, the acid-base etching waste liquid inlet is respectively connected with the etching waste liquid outlet of an acidic etching production line 14 and the etching waste liquid outlet of an alkaline etching production line 15, the neutralized etching waste liquid outlet is connected with the cuprous chloride filtering and recovering device 12, the cuprous chloride filtering and recovering device 12 is provided with a filtered etching waste liquid outlet and a cuprous chloride precipitate outlet, the filtered etching waste liquid outlet is connected with the acid-base etching liquid regenerating device 13, the etching liquid regenerating device 13 is respectively connected with the acidic etching production line 14 and the alkaline etching production line 15, the cuprous chloride precipitate outlet is respectively connected with the cuprous chloride purification system 2 and the electrolytic copper extraction recovery system 3, and the etching waste liquid collecting and the PH value detecting device 11. In this embodiment, the cuprous chloride filtering and recovering device can collect the acid-base etching waste liquid, neutralize the etching waste liquid in the device, separate the neutralized etching waste liquid from the cuprous chloride precipitate, treat and adjust the neutralized etching waste liquid into new acid-base etching liquid through the acid-base etching liquid regeneration device, provide the new acid-base etching liquid for etching production of an etching production line, purify and recover the cuprous chloride precipitate into a cuprous chloride finished product through the cuprous chloride purification system, recover the cuprous chloride precipitate into a copper finished product through the electrolysis copper extraction recovery system, precipitate a cuprous chloride precipitate crude product through neutralization of the acid etching waste liquid and the alkaline etching waste liquid, do not need to add any additive, the etching waste liquid does not enter the copper extraction equipment, and does not bring impurities, the etching waste liquid is easy to regenerate and circulate, the quality of the regenerated acid-base etching liquid is obviously improved, the using amount only needs 1/5 of the acid-base etching liquid regenerated by the existing process, the production material cost is effectively reduced, different recycling systems of the acid-base etching waste liquid are integrated into a set of recycling system, the equipment floor area is small, and the equipment cost is low; the crude cuprous chloride precipitate can be purified and processed into a cuprous chloride finished product, the purity is up to more than 99%, the purification process only has a small amount of volatile matters of hydrochloric acid and ethanol, the tail gas treatment cost is low, and the production cost is reduced; the crude cuprous chloride precipitate can also be dissolved for electrolytic copper extraction, and the copper ions in the etching waste liquid can be treated from 100g per liter to 5g-10g per liter, so that the extraction efficiency of copper is greatly improved.
As shown in fig. 1, the acid-base etching waste liquid collecting and neutralizing device 11 includes an alkaline etching waste liquid collecting tank 111, an acidic etching waste liquid collecting tank 112, and an acid-base etching waste liquid neutralizing tank 113, where the acid-base etching waste liquid neutralizing tank 113 is respectively communicated with the alkaline etching waste liquid collecting tank 111 and the acidic etching waste liquid collecting tank 112, the neutralizing etching waste liquid outlet is fixedly disposed on the acid-base etching waste liquid neutralizing tank 113, the acid-base etching waste liquid inlet includes an acidic etching waste liquid inlet and an alkaline etching waste liquid inlet, the alkaline etching waste liquid collecting tank 111 is communicated with an etching waste liquid outlet of the alkaline etching production line 15 through the alkaline etching waste liquid inlet, and the acidic etching waste liquid collecting tank 112 is communicated with an etching waste liquid outlet of the acidic etching production line 14 through the acidic etching waste liquid inlet; the cuprous chloride filtering and recycling device 12 comprises a cuprous chloride filter tank 121, a drainage port of the filtered etching waste liquid is arranged on the side surface of the bottom of the cuprous chloride filter tank 121, a drainage port of cuprous chloride precipitate is arranged at the bottom of the cuprous chloride filter tank 121, and a water outlet of the neutralized etching waste liquid is communicated with the cuprous chloride filter tank 121; the acid-base etching solution regeneration device 13 comprises a regeneration solution collection tank 131, an acid etching solution regenerator 132, an alkaline etching solution regenerator 133, an acid etching solution electronic tank 134 and an alkaline etching solution tank 135 which are fixedly connected in sequence, wherein the regeneration solution collection tank 131 is communicated with a filtered etching waste solution discharge port, the regeneration solution collection tank 131 is respectively communicated with the acid etching solution regenerator 132 and the alkaline etching solution regenerator 133, the acid etching solution regenerator 132 is communicated with the acid etching solution electronic tank 134, the alkaline etching solution regenerator 133 is communicated with the alkaline etching solution electronic tank 135, the acid etching solution electronic tank 134 is communicated with the acid etching production line 14, and the alkaline etching solution electronic tank 135 is communicated with the alkaline etching production line 15; the additive added to the etching waste liquid in the acidic etching liquid regenerator 132 is hydrochloric acid, and the additive added to the etching waste liquid in the alkaline etching liquid regenerator 133 is ammonia water.
In this embodiment, as shown in fig. 6, fig. 6 is a table showing the content of copper ions before and after filtration by the etching waste liquid recycling system of the present invention, and by utilizing the characteristic that cuprous chloride, which is a main component of the acid-base etching waste liquid, is precipitated in a neutral PH value, the etching waste liquids in the acidic etching production line and the alkaline etching production line are neutralized in the acid-base etching waste liquid neutralization tank, and the cuprous chloride is precipitated by neutralizing the acid-base etching waste liquid, so as to filter out a crude cuprous chloride product; sending the filtered etching waste liquid into a regeneration liquid collecting tank, then respectively sending the waste liquid into an acidic etching liquid regenerator and an alkaline etching liquid regenerator, adding hydrochloric acid and an additive into the waste liquid at the moment of sending the waste liquid into the acidic etching liquid regenerator, and sending the waste liquid into an acidic etching liquid tank for etching production of an acidic etching production line; and adding ammonia water and additives into the waste liquid at the moment of sending the waste liquid into the alkaline etching liquid regenerator, blending the waste liquid and then sending the waste liquid into an alkaline etching liquid tank for etching production of an alkaline etching production line. The main chemical principle of the neutralization of the etching waste liquid in the acid-base etching waste liquid neutralization tank is as follows:
acid complexation, cuCl + HCl = H [ CuCl2];
basic complexation reaction, cuCl +2NH 3. H2O =2H2O + [ Cu (NH 3) 2] cl;
acid-base neutralization complex breaking reaction, 2H2 [ CuCl2] + [ Cu (NH 3) 2] <' > Cl =2CuCl ↓ +2NH4Cl +2H2O. .
As shown in fig. 2, the cuprous chloride purification system 2 includes a dilute hydrochloric acid cleaning tank 21, a dilute hydrochloric acid filtering tank 22, an ethanol cleaning tank 23 and an ethanol filtering tank 24, which are fixedly connected in sequence, the cuprous chloride precipitate discharge port is communicated with the dilute hydrochloric acid cleaning tank 21, the dilute hydrochloric acid filtering tank 22 is provided with a cuprous chloride hydrochloric acid cleaning discharge port and a dilute hydrochloric acid filtrate discharge port, the cuprous chloride hydrochloric acid cleaning discharge port is communicated with the ethanol cleaning tank 23, the dilute hydrochloric acid filtrate discharge port is communicated with the dilute hydrochloric acid cleaning tank 21, the ethanol filtering tank 24 is provided with a cuprous chloride finished product discharge port and an ethanol filtrate discharge port, and the ethanol filtrate discharge port is communicated with the ethanol cleaning tank 23. In the embodiment, a cuprous chloride finished product with the purity of more than 99% can be obtained by cleaning and purifying a cuprous chloride crude product by utilizing the principle that cuprous chloride is insoluble in dilute hydrochloric acid and ethanol, the purification process only has a small amount of volatile matters of hydrochloric acid and ethanol, the tail gas treatment cost is low, and the production cost is reduced.
As shown in fig. 3, the electrolytic copper extraction recovery system 3 is an extraction electrolytic copper extraction system 4, and includes a cuprous chloride crude product extraction dissolving tank 41, an alkaline extraction high copper solution collecting tank 42, an alkaline extraction low copper solution collecting tank 43, and an extraction copper extraction device 44, wherein the cuprous chloride crude product extraction dissolving tank 41 is respectively communicated with a cuprous chloride precipitate discharge port and the alkaline extraction high copper solution collecting tank 42, the alkaline extraction high copper solution collecting tank 42 is communicated with the extraction copper extraction device 44, the extraction copper extraction device 44 is communicated with the alkaline extraction low copper solution collecting tank 43, the alkaline extraction low copper solution collecting tank 43 is communicated with the cuprous chloride crude product extraction dissolving tank 41, the extraction copper extraction device 44 includes an extraction tank 441, a rinsing tank 442, a stripping tank 443, and a copper recovery electrolytic tank 444, the extraction tank 441 is respectively communicated with the alkaline extraction high copper solution collecting tank 42 and the alkaline extraction low copper solution collecting tank 43, and the extraction tank 441, the rinsing tank 442, the stripping tank 443, and the copper recovery electrolytic tank 444 are sequentially and fixedly connected. In this embodiment, the cuprous chloride precipitate crude product is dissolved in the cuprous chloride crude product extraction dissolving tank and then sent to the alkaline extraction high copper solution collecting tank, the alkaline high copper solution in the alkaline extraction high copper solution collecting tank can be extracted in the extraction tank, and the extracted copper solution can flow into the rinsing tank to wash off the residual alkaline high copper solution and then flow into the back extraction tank to complete back extraction, and then flow into the copper recovery electrolytic tank to perform copper electrolysis.
As shown in fig. 4, the electrolytic copper extraction recovery system 3 is an alkaline direct electrolytic copper extraction system 5, and includes a cuprous chloride crude product alkaline dissolving tank 51, an alkaline electrolytic copper extraction high copper solution collecting tank 52, an alkaline electrolytic copper extraction low copper solution collecting tank 53 and an alkaline direct electrolytic copper extraction solution tank 54, wherein the cuprous chloride crude product alkaline dissolving tank 51, the alkaline electrolytic copper extraction high copper solution collecting tank 52, the alkaline electrolytic copper extraction low copper solution collecting tank 54 and the alkaline direct electrolytic copper extraction solution tank 54 are sequentially and fixedly communicated, and the alkaline direct electrolytic copper extraction solution tank 54 is further communicated with the cuprous chloride crude product alkaline dissolving tank 51. In this embodiment, the cuprous chloride precipitate crude product is dissolved in the cuprous chloride crude product alkaline dissolving tank and then sent to the alkaline electrolysis copper extraction high copper solution collecting tank, and the alkaline high copper solution in the alkaline electrolysis copper extraction high copper solution collecting tank can flow into the alkaline direct electrolysis copper extraction solution tank to perform electrolysis copper extraction.
As shown in fig. 5, the electrolytic copper-extracting recovery system 4 is an acidic direct film electrolytic copper-extracting system 6, which includes an acidic cuprous chloride crude product dissolution tank 61, an acidic electrolytic copper-extracting high copper solution collection tank 62, an acidic electrolytic copper-extracting low copper solution collection tank 63 and an acidic direct film electrolytic copper-extracting solution tank 64, wherein the acidic cuprous chloride crude product dissolution tank 61, the acidic electrolytic copper-extracting high copper solution collection tank 62, the acidic electrolytic copper-extracting low copper solution collection tank 63 and the acidic direct film electrolytic copper-extracting solution tank 64 are sequentially and fixedly communicated, and the acidic direct electrolytic copper-extracting solution tank 64 is further communicated with the cuprous chloride crude product acidic dissolution tank 61 and the acidic etching production line 24. In the embodiment, the cuprous chloride precipitate crude product is dissolved in an acidic cuprous chloride crude product dissolving tank and then is sent to an acidic electrolytic copper-extracting high-copper solution collecting tank, and the acidic high-copper solution in the acidic electrolytic copper-extracting high-copper solution collecting tank can flow into an acidic direct-film electrolytic copper-extracting solution tank to perform electrolytic copper extraction.
According to the etching waste liquid recycling and cuprous chloride and copper recovery system, the etching waste liquid recycling system, the cuprous chloride purification system and the electrolytic copper extraction recovery system which are matched with each other are arranged in the etching waste liquid recycling system, the cuprous chloride filtering and recovering device can separate the neutralized etching waste liquid from cuprous chloride precipitates after the acid-base etching waste liquid is collected and neutralized in the neutralizing device, the neutralized etching waste liquid is treated and adjusted into new acid-base etching liquid by the acid-base etching liquid regeneration device and is supplied to etching production lines for etching production, the cuprous chloride precipitates are purified and recovered into cuprous chloride finished products by the cuprous chloride purification system, the cuprous chloride precipitates are recovered into copper finished products by the electrolytic copper extraction recovery system, the cuprous chloride precipitated crude products can be precipitated by neutralizing the acidic etching waste liquid and the alkaline etching waste liquid, no additive is needed, the etching waste liquid does not enter the copper extraction equipment, impurities cannot be brought in, the etching waste liquid is easy to be recycled, the quality of the regenerated acid-base etching liquid is obviously improved, the consumption of the acid-base etching liquid which is 1/5 of the regenerated by the existing process is used, the production material cost is effectively reduced, the acid-base etching waste liquid recycling system is integrated into a small recycling system, and the regeneration system is integrated with low cost; the crude cuprous chloride precipitate can be purified and processed into a cuprous chloride finished product, the purity is up to more than 99%, the purification process only has a small amount of volatile matters of hydrochloric acid and ethanol, the tail gas treatment cost is low, and the production cost is reduced; the crude cuprous chloride precipitate can also be dissolved for electrolytic copper extraction, the copper ions in the etching waste liquid can be treated from 100g per liter to 5g-10g per liter, the extraction efficiency of copper is greatly improved, and the problems that in the current etching production line, the etching waste liquid needs to be provided with different recycling regeneration equipment, the current copper extraction process efficiency is not high, the etching liquid quality of the current etching waste liquid recycling regeneration system is low, and the current cuprous chloride production cost is high are solved.
The above-described embodiments are intended to be illustrative, and not restrictive, of the invention, and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. The utility model provides an etching waste liquid circulation regeneration and cuprous chloride, copper recovery system which characterized in that: the copper chloride waste liquor recycling system comprises an acid-base etching waste liquor collecting neutralization device, a cuprous chloride filtering and recycling device and an acid-base etching waste liquor recycling device which are fixedly connected in sequence, wherein the acid-base etching waste liquor collecting neutralization device is provided with an acid-base etching waste liquor water inlet and a neutralized etching waste liquor water outlet, the acid-base etching waste liquor water inlet is connected with an etching waste liquor outlet of an acid etching production line and an etching waste liquor outlet of an alkaline etching production line respectively, the neutralized etching waste liquor water outlet is connected with the cuprous chloride filtering and recycling device, the cuprous chloride filtering and recycling device is provided with a filtered etching waste liquor outlet and a cuprous chloride precipitate outlet, the filtered etching waste liquor outlet is connected with the acid-base etching waste liquor recycling device, the acid-base etching waste liquor recycling device is further connected with the acid etching production line and the alkaline etching production line respectively, the cuprous chloride precipitate outlet is connected with the cuprous chloride purifying and recycling system, the electrolysis copper extracting and recycling system is connected with the acid-base etching waste liquor collecting neutralization device, the cuprous chloride filtering and recycling device can adjust the pH value of the etching waste liquor and the copper chloride precipitate and the acid-base etching waste liquor collecting neutralization device and the acid-base etching waste liquor and the copper chloride precipitate recycling device and the finished product.
2. The etching waste liquid recycling and cuprous chloride and copper recovering system according to claim 1, wherein said system comprises: acid-base etching waste liquid is collected neutralization apparatus includes alkaline etching waste liquid collection tank, acid etching waste liquid collection tank and acid-base etching waste liquid neutralization jar, acid-base etching waste liquid neutralization jar respectively with alkaline etching waste liquid collection tank acid etching waste liquid collection tank intercommunication, neutralization etching waste liquid delivery port fixed set up in the acid-base etching waste liquid neutralization jar on, acid-base etching waste liquid water inlet includes acid etching waste liquid water inlet and alkaline etching waste liquid water inlet, alkaline etching waste liquid collection tank passes through alkaline etching waste liquid water inlet with the etching waste liquid export intercommunication of alkaline etching production line, acid etching waste liquid collection tank passes through acid etching waste liquid water inlet with the etching waste liquid export intercommunication of acid etching production line.
3. The etching waste liquid recycling and cuprous chloride and copper recovering system according to claim 2, wherein said system comprises: cuprous chloride filters recovery unit includes the cuprous filter-tank, the back etching waste liquid outlet of straining set up in cuprous filter-tank bottom side, cuprous chloride precipitate discharge port set up in cuprous filter-tank bottom, neutralization etching waste liquid delivery port with the cuprous filter-tank intercommunication.
4. The etching waste liquid recycling and cuprous chloride and copper recovering system according to claim 3, wherein said system comprises: acid-base etching liquid regenerating unit is including fixed connection's regeneration liquid collection tank, acid etching liquid regenerator, basicity etching liquid regenerator, acid etching liquid tank and basicity etching liquid tank in proper order, the regeneration liquid collection tank with strain back etching waste liquid outlet intercommunication, the regeneration liquid collection tank respectively with acid etching liquid regenerator basicity etching liquid regenerator intercommunication, acid etching liquid regenerator with acidity etching liquid tank intercommunication, basicity etching liquid regenerator with basicity etching liquid tank intercommunication, acid etching liquid tank with basicity etching production line intercommunication.
5. The etching waste liquid recycling and cuprous chloride and copper recovering system according to claim 4, wherein said system comprises: the additive added to the etching waste liquid in the acidic etching liquid regenerator is hydrochloric acid, and the additive added to the etching waste liquid in the alkaline etching liquid regenerator is ammonia water.
6. The etching waste liquid recycling and cuprous chloride and copper recovering system according to claim 5, wherein said system comprises: cuprous chloride purification system washs jar, dilute hydrochloric acid filter-tank, ethanol washing jar and ethanol filter-tank including the dilute hydrochloric acid of fixed connection in proper order, cuprous chloride precipitate discharge port with dilute hydrochloric acid washs jar intercommunication, dilute hydrochloric acid filter-tank is equipped with cuprous chloride hydrochloric acid washing discharge port and dilute hydrochloric acid filtrate outlet, cuprous chloride hydrochloric acid washing discharge port with ethanol washing jar intercommunication, dilute hydrochloric acid filtrate outlet with dilute hydrochloric acid washs jar intercommunication, the ethanol filter-tank is equipped with cuprous chloride finished product discharge port and ethanol filtrate outlet, ethanol filtrate outlet with ethanol washing jar intercommunication.
7. The system for recycling etching waste liquid and recovering cuprous chloride and copper according to claim 6, wherein said system comprises: copper recovery system is carried for extraction electrolysis to electrolysis carries copper system, including cuprous chloride crude extraction dissolving tank, alkaline extraction high copper solution collecting vessel, alkaline extraction low copper solution collecting vessel and extraction and carry the copper device, cuprous chloride crude extraction dissolving tank respectively with cuprous chloride precipitate discharge port alkaline extraction high copper solution collecting vessel intercommunication, alkaline extraction high copper solution collecting vessel with copper device intercommunication is carried in the extraction, the extraction carry the copper device with alkaline extraction low copper solution collecting vessel intercommunication, alkaline extraction low copper solution collecting vessel with cuprous chloride crude extraction dissolving vessel intercommunication.
8. The etching waste liquid recycling and cuprous chloride and copper recovering system according to claim 7, wherein said system comprises: the copper device is carried in extraction includes extraction tank, rinsing bath, back extraction groove and copper recovery electrolysis trough, the extraction tank respectively with the high copper solution collector tank of alkaline extraction the low copper solution collector tank intercommunication of alkaline extraction, the extraction tank the rinsing bath back extraction groove with the copper recovery electrolysis trough is fixed connection in proper order, the high copper solution of alkaline in the high copper solution collector tank of alkaline extraction can by the extraction in the extraction tank, the extraction copper solution can flow in the rinsing bath washes off and remains the high copper solution of alkaline and flow in again the back extraction groove is accomplished and is flowed in after the back extraction the copper is carried in the electrolysis in the copper recovery electrolysis trough.
9. The etching waste liquid recycling and cuprous chloride and copper recovering system according to claim 6, wherein said system comprises: copper recovery system is carried to electrolysis carries copper system for alkaline direct electrolysis, carry the copper high copper solution collecting vessel, alkaline electrolysis including cuprous chloride crude basicity dissolving tank, alkaline electrolysis and carry the copper low copper solution collecting vessel and alkaline direct electrolysis and carry the copper solution groove, cuprous chloride crude basicity dissolving tank the copper high copper solution collecting vessel is carried to alkaline electrolysis the copper low copper solution collecting vessel is carried to alkaline electrolysis with copper solution groove is carried to alkaline direct electrolysis fixed intercommunication in proper order, alkaline direct electrolysis carry the copper solution groove still with cuprous chloride crude basicity dissolving tank intercommunication.
10. The etching waste liquid recycling and cuprous chloride and copper recovering system according to claim 6, wherein said system comprises: copper recovery system is carried to electrolysis carries copper system for acid direct film electrolysis, carry the high copper solution collecting vessel of copper, acid electrolysis including cuprous chloride crude acid dissolving tank, acid electrolysis and carry the low copper solution collecting vessel of copper and acid direct film electrolysis and carry the copper solution groove, cuprous chloride crude acid dissolving tank the high copper solution collecting vessel of copper is carried to acid electrolysis the low copper solution collecting vessel of copper is carried to acid electrolysis with the copper solution groove is carried to acid direct film electrolysis is fixed the intercommunication in proper order, the copper solution groove is carried to acid direct electrolysis still with cuprous chloride crude acid dissolving tank acid etching production line intercommunication.
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| CN202211591722.XA CN115928078A (en) | 2022-12-12 | 2022-12-12 | Etching waste liquid cyclic regeneration and cuprous chloride, copper recovery system |
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