CN113549773A - Process for producing high-purity sponge copper by using copper chloride acidic etching waste liquid - Google Patents
Process for producing high-purity sponge copper by using copper chloride acidic etching waste liquid Download PDFInfo
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- CN113549773A CN113549773A CN202110811960.6A CN202110811960A CN113549773A CN 113549773 A CN113549773 A CN 113549773A CN 202110811960 A CN202110811960 A CN 202110811960A CN 113549773 A CN113549773 A CN 113549773A
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- copper
- acidic etching
- copper chloride
- etching solution
- waste liquid
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions
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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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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- ing And Chemical Polishing (AREA)
Abstract
The invention relates to the technical field of sponge copper production, in particular to a process for producing high-purity sponge copper by using copper chloride acidic etching waste liquid, which comprises the following steps: s1, water distribution: at 10m3Adding copper chloride acid etching solution into the reaction kettle, and adding 10m3The method comprises the steps of replacing the copper chloride acidic etching solution by using the copper chloride acidic etching waste liquid to obtain high-purity sponge copper, wherein the copper content is about 90 percent, the water content is about 10 percent, the iron content is stabilized at 0.3 to 1 percent, and the total content of other impurities is less than 0.5 percent, so that the prepared sponge copper is high in quality and activity, and can be directly used as a raw material to prepare other copper salt products, and the copper chloride acidic etching solution is used for preparing other copper salt products, so that the copper chloride acidic etching solution is uniformly stirred by adding water until the copper content reaches a proper concentration rangeThe high-purity sponge copper produced by the copper acidic etching solution has the advantages of high recovery rate, simple process and low manufacturing cost, and is more suitable for large-scale popularization and use.
Description
Technical Field
The invention relates to the technical field of sponge copper production, in particular to a process for producing high-purity sponge copper by utilizing copper chloride acidic etching waste liquid.
Background
The PCB (printed circuit board) industry in China is developed, the first manufacturing country in the world is, the PCB yield and the PCB output value are all located in the world, a large amount of copper-containing etching waste liquid can be generated in the PCB production process, the content of pollutants such as copper, iron and acid in the waste liquid is very high, if the waste liquid is directly discharged, water bodies can be seriously polluted, environmental pollution and ecological damage are caused, resources are greatly wasted, the concentration of the pollutants in the waste liquid can be reduced to the range allowed by the discharge standard through recycling, and huge economic value is obtained.
The comprehensive recovery and utilization technology of the acidic etching solution mainly extracts copper ions in the acidic etching solution, other components are not basically extracted, and metal copper has higher value, so the most basic treatment of the acidic etching solution is to recover the metal copper from the acidic etching waste solution, the purity of the sponge copper obtained by a metal replacement method is generally 70%, the recovery rate is 85%, the purity of the recovered copper is low, and the recovery rate is low.
In conclusion, the invention solves the existing problems by designing a process for producing high-purity sponge copper by using the acidic copper chloride etching waste liquid.
Disclosure of Invention
The invention aims to provide a process for producing high-purity sponge copper by using copper chloride acidic etching waste liquid, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a process for producing high-purity sponge copper by utilizing copper chloride acidic etching waste liquid comprises the following steps:
s1, water distribution: at 10m3Adding copper chloride acid etching solution into the reaction kettle, and adding 10m3Adding water into the copper chloride acidic etching solution in the reaction kettle, stirring uniformly, when the copper content reaches a proper concentration range, adding water into the copper chloride acidic etching solution, replacing,
s2, substitution: adding iron powder of above 600 meshes for replacement, continuously stirring for reaction, filtering by a filter press after reaction,
s3, dilution: and then tap water is used for cleaning until no ferrous ion is detected in the filtrate, and a high-purity sponge copper product is obtained.
In a preferable embodiment of the invention, the stirring speed in S1 is 150 to 200r/min, and the copper chloride acidic etching solution is mixed with water until the copper content reaches a proper concentration range of 5.5 to 6.5%.
In a preferable embodiment of the invention, the stirring reaction speed of S2 is 150-200 r/min, and the stirring is continued for 3-4 h.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the high-purity sponge copper is obtained by adopting the copper chloride acidic etching waste liquid for replacement, the copper content reaches about 90%, the water content is about 10%, the iron content is stabilized at 0.3% -1%, and the total content of the other impurities is less than 0.5%, so that the prepared sponge copper has high quality and high activity, and can be directly used as a raw material for preparing other copper salt products, and thus, the high-purity sponge copper produced by using the copper chloride acidic etching liquid has the advantages of high recovery rate, simple process and low manufacturing cost, and is more suitable for large-scale popularization and application.
Drawings
FIG. 1 is a schematic view of the process flow structure of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
While several embodiments of the present invention will be described more fully hereinafter with reference to the accompanying drawings, in order to facilitate an understanding of the invention, the invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed to provide a more complete disclosure of the invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present, that when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present, and that the terms "vertical", "horizontal", "left", "right" and the like are used herein for descriptive purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in the specification of the present invention are for the purpose of describing particular embodiments only and are not intended to limit the present invention, and the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, the present invention provides a technical solution:
a process for producing high-purity sponge copper by utilizing copper chloride acidic etching waste liquid comprises the following steps:
s1, water distribution: at 10m3Adding copper chloride acid etching solution into the reaction kettle, and adding 10m3Adding water into the copper chloride acidic etching solution in the reaction kettle, stirring uniformly, when the copper content reaches a proper concentration range, adding water into the copper chloride acidic etching solution, replacing,
s2, substitution: adding iron powder of above 600 meshes for replacement, continuously stirring for reaction, filtering by a filter press after reaction,
s3, dilution: and then tap water is used for cleaning until no ferrous ion is detected in the filtrate, and a high-purity sponge copper product is obtained.
In a further preferable embodiment of the invention, the stirring speed in S1 is 150 to 200r/min, and the copper chloride acidic etching solution is distributed with water until the copper content reaches a suitable concentration range of 5.5 to 6.5%.
In a further preferable embodiment of the present invention, the stirring reaction speed of S2 is 150 to 200r/min, and the stirring is continued for 3 to 4 hours.
The specific implementation case is as follows:
at 10m35.0t of copper chloride acid etching solution, 9.97 percent of copper, 11.38 percent of hydrochloric acid and 3.1t of water are added into a reaction kettle, the mixture is uniformly stirred at the speed of 150r/min, 178kg of 600-mesh iron powder is slowly added into the reaction kettle under the stirring speed of 150r/min, the reaction lasts for 3h until no copper ions are contained in the material solution, the material solution is filter-pressed by a filter press, the sponge copper is washed by tap water until no ferrous ions are contained in the washing water, the filter cake is naturally dried until no water drips to obtain high-purity sponge copper, the sponge copper is sampled and tested, the copper content is 88.72 percent, the water content is 10.20 percent, the iron content is 0.82 percent, and therefore, the high-purity sponge copper is obtained by replacing the copper chloride acid etching waste liquid, the copper content reaches about 90 percent, the water content is about 10 percent, the iron content is stabilized at 0.3 to 1 percent, and the total content of other impurities is less than 0.5 percent, so that the quality of the prepared sponge copper is high, the activity is high, and other copper salt products can be directly prepared by taking the copper chloride acid etching solution as a raw material, so that the high-purity sponge copper produced by using the copper chloride acid etching solution has the advantages of high recovery rate, simple process and low manufacturing cost, and is more suitable for large-scale popularization and application.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A process for producing high-purity sponge copper by utilizing copper chloride acidic etching waste liquid comprises the following steps:
s1, water distribution: at 10m3Adding copper chloride acid etching solution into the reaction kettle, and adding 10m3Adding water into the copper chloride acidic etching solution in the reaction kettle, stirring uniformly, when the copper content reaches a proper concentration range, adding water into the copper chloride acidic etching solution, replacing,
s2, substitution: adding iron powder of above 600 meshes for replacement, continuously stirring for reaction, filtering by a filter press after reaction,
s3, dilution: and then tap water is used for cleaning until no ferrous ion is detected in the filtrate, and a high-purity sponge copper product is obtained.
2. The process for producing high-purity sponge copper by utilizing the copper chloride acidic etching waste liquid as claimed in claim 1, which is characterized in that: and in the S1, the stirring speed is 150-200 r/min, and the copper chloride acidic etching solution is distributed with water until the copper content reaches a proper concentration range of 5.5-6.5%.
3. The process for producing high-purity sponge copper by utilizing the copper chloride acidic etching waste liquid as claimed in claim 1, which is characterized in that: and the stirring reaction speed of the S2 is 150-200 r/min, and the stirring is continuously carried out for 3-4 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202110811960.6A CN113549773A (en) | 2021-07-19 | 2021-07-19 | Process for producing high-purity sponge copper by using copper chloride acidic etching waste liquid |
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| CN202110811960.6A CN113549773A (en) | 2021-07-19 | 2021-07-19 | Process for producing high-purity sponge copper by using copper chloride acidic etching waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114317980A (en) * | 2021-12-30 | 2022-04-12 | 韶关绿鑫环保技术有限公司 | Sponge copper and production process thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818385A (en) * | 2015-04-10 | 2015-08-05 | 吴江市松陵镇氧化铜厂 | Energy-saving, environmental-protection and zero-discharge technology of acidic waste etching solution resource recycling treatment |
| CN110218878A (en) * | 2019-07-01 | 2019-09-10 | 陕西安信显像管循环处理应用有限公司 | A kind of method of acidic etching liquid displacement production frerrous chloride |
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- 2021-07-19 CN CN202110811960.6A patent/CN113549773A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818385A (en) * | 2015-04-10 | 2015-08-05 | 吴江市松陵镇氧化铜厂 | Energy-saving, environmental-protection and zero-discharge technology of acidic waste etching solution resource recycling treatment |
| CN110218878A (en) * | 2019-07-01 | 2019-09-10 | 陕西安信显像管循环处理应用有限公司 | A kind of method of acidic etching liquid displacement production frerrous chloride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114317980A (en) * | 2021-12-30 | 2022-04-12 | 韶关绿鑫环保技术有限公司 | Sponge copper and production process thereof |
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