CN109911928B - Method for quickly dissolving copper - Google Patents
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- CN109911928B CN109911928B CN201910214462.6A CN201910214462A CN109911928B CN 109911928 B CN109911928 B CN 109911928B CN 201910214462 A CN201910214462 A CN 201910214462A CN 109911928 B CN109911928 B CN 109911928B
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Abstract
The invention discloses a method for quickly dissolving copper, which is characterized in that solid copper is added into a copper dissolving tank through a copper material adding port, the material accumulation thickness is proper for air to smoothly pass through, and a material adding port is closed after the material is added; starting a circulating pump to add the dissolving solution into the copper dissolving tank 1 through a dissolving solution inlet; starting a heating device, heating the dissolved solution to 50-65 ℃, adding compressed air into the dissolved copper tank 1, adding SO2 gas through an SO2 gas inlet, comprehensively adjusting various reaction parameters, quickly dissolving copper to generate CuSO4, stopping the reaction when the concentration of Cu2+ in the solution is more than or equal to 100g/L, discharging the solution through a dissolved solution discharge port of the dissolved copper tank, discharging the produced qualified copper sulfate solution through a dissolved solution outlet, and discharging waste gas through an exhaust port. The invention has the advantages of high copper dissolution rate, utilization rate of oxygen in the air of 80 percent, great reduction of the amount of blown air, reduction of the evaporation capacity of the dissolution liquid of about 30 percent and copper dissolution capacity of 800kg/m3. d.
Description
Technical Field
The invention belongs to the field of chemical industry, relates to recycling of waste copper, and particularly relates to a method for quickly dissolving copper.
Background
Dissolving copper is to change solid copper into Cu2+And the copper salt is dissolved in aqueous solution and widely applied to copper sulfate preparation, copper foil production and copper salt preparation by recovering waste copper. Air is used as oxidant in both domestic and foreign copper dissolution, and during the production process, the air is filled into the dissolution liquid and then reacts with the metal copper. Air (mainly oxygen in the air) is used as an oxidant, the oxidation potential is lower and is only 400-500mV, the copper dissolution speed is slow, the reaction time is long, and the production efficiency is low.
Disclosure of Invention
Aiming at the problems existing in the existing copper dissolution, the invention provides a method for quickly dissolving copper, which shortens the reaction time, reduces the reaction temperature and the production cost and improves the copper dissolution efficiency.
The technical scheme adopted by the invention is as follows: a method for quickly dissolving copper comprises the following steps,
a. adding solid copper and a dissolving solution into a copper dissolving tank in sequence, wherein the dissolving solution is a mixed solution prepared from sulfuric acid and copper sulfate, the sulfuric acid concentration in the mixed solution is 30-180g/L, and the Cu concentration in the mixed solution is 30-180g/L2+The initial concentration is 0-55 g/L;
b. heating the solution to 50-65 deg.C, stopping heating, introducing 0.03-0.3Mpa compressed air into the solution from the bottom of copper dissolving tank at flow rate of 5-550m3H, introducing 0.035-0.35Mpa into the compressed air before the compressed air enters the dissolving tank, and the flow rate is 0.15-55 m3SO of/h2Gas, compressed air and SO2The volume ratio of the gas to the gas is 100: 3-10, increasing the oxidation potential of the solution, and quickly oxidizing the dissolved copper to generate CuSO4。
The solid copper is any one of copper blocks, copper grains, copper wires and copper powder.
Preferably, the mixed solution contains 80-90g/L of sulfuric acid and Cu2+The initial concentration is 15-25 g/L.
Preferably, SO is introduced into the compressed air before the compressed air enters the dissolving tank2The pressure of the gas is higher than the pressure of the compressed air.
Preferably, the amount of the dissolving solution is 2.9-4.5m per ton of solid copper3And (6) counting.
The volume of the dissolving solution is determined according to production requirements, and when the volume is insufficient, the dissolving solution tank is independently arranged and is connected with the copper dissolving tank in series for use; when the copper content in the dissolving solution is high, a plurality of copper dissolving tanks are connected in series for use.
The invention introduces compressed air and SO2The oxidation potential of the dissolved solution after the gas is increased from 500mV of 400 to 1200mV of 1000.
When the concentration of Cu2+ in the solution exceeds or equals to 100g/L, the reaction is stopped and the solution is discharged through a dissolved solution discharge port of a dissolved copper tank.
Preferably, the volume of the copper dissolving tank is 3-120m3And the height is 3-6 m. And a plurality of discharging layers for placing solid copper are arranged in the copper dissolving tank.
Compared with the existing copper dissolving method, the method has the following advantages:
1. adding SO accounting for 3-10% of the volume of compressed air before adding air into a copper dissolving tank2The oxidation potential of the solution is increased from 400-1200 mV to 1000-1200mV (namely, SO)2Dissolved in water and separated out SO3 2-；SO3 2-With O in air2Combined to form SO5 2-，SO5 2-Has high energy groups, and the oxidation potential of the dissolving solution can reach 1200mV at most. ) The oxidation efficiency is improved by more than 2 times, and the copper is quickly dissolved to generate CuSO4The utilization rate of oxygen in the air reaches 80 percent, the amount of blown air is greatly reduced, the evaporation amount of the dissolving solution is reduced by about 30 percent, and the copper dissolving capacity can reach 800kg/m3.d。
2.SO2Adding the solution and air to generate sulfuric acid, reacting with Cu to generate CuSO4No excessive substance is generated in the dissolving solution, no side reaction is generated, and the consumption of sulfuric acid can be reduced.
2. The invention solves the defects of low oxidation potential, low copper dissolution speed, long reaction time and low production efficiency when air and oxygen are used as oxidants.
3. The invention has high oxidation potential of the dissolving solution, high copper dissolving speed, more heat released in unit time and no need of heating the dissolving solution in the copper dissolving process.
4. When the copper is dissolved, the production efficiency is low due to the excessively low temperature, the dissolved amounts of oxygen and other gases in the dissolved solution are rapidly reduced when the temperature exceeds 80 ℃, and the production speed is greatly slowed down; because the solid copper is dissolved to be an exothermic reaction, the method only needs to heat the dissolved solution to 50-65 ℃ at the initial stage of production and then stop heating, the oxidation potential of the dissolved solution is high, and the solid copper can be dissolved to quickly react at the low temperature of 50-60 ℃; the invention has high oxidation potential of the dissolving solution, so that the dissolving speed of copper is still high even if the concentration of sulfuric acid is 20 g/L.
5. Hair brushThe volume of the bright copper dissolving tank is determined according to production requirements, and is generally 3-120m3And the height is between 3 and 6 m; through set up a plurality of solid copper material layers in dissolving the copper jar, increase solid copper charge capacity, with piling up on every layer of solid copper, thickness uses mist to pass through smoothly as the standard, has increased with the air, and has dissolved the area of contact of liquid for reaction rate has shortened production cycle.
6. The solid copper can be copper blocks, copper rice, copper wires, copper powder and the like, the specific surface area is increased by shearing the solid copper, and the larger the specific surface area is, the larger the reaction area is, the higher the dissolving speed is and the higher the production efficiency is.
7. In the invention, SO2The gas is added before the air enters the dissolving tank, SO that the air and SO are convenient to be mixed2Mixing thoroughly, and compressing air and SO2The volume ratio of the gas is set as 100: 3-10 solid copper has high dissolution rate due to SO2The gas concentration is too low, the solution has weak oxidizability and SO2The solution with too high gas concentration is reductive, and the dissolution speed is reduced sharply.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
In the figure: 1. a copper dissolving tank; 2. an air inlet; 3. SO (SO)2A gas inlet; 4. a dissolved solution outlet; 5. a dissolving liquid inlet; 6. a copper material feeding port; 7. an air outlet.
Detailed Description
A method for quickly dissolving copper comprises the following steps: solid copper (copper blocks, copper wires, copper sheets and copper powder) is added into the copper dissolving tank 1 through a copper material adding port 6, the material accumulation thickness is proper for air to smoothly pass through, and the material adding port is closed after the material adding is finished; starting a circulating pump to add the dissolving solution into the copper dissolving tank 1 through a dissolving solution inlet 5; starting heating equipment to heat the solution; compressed air (oxygen) is added into the copper dissolving tank 1 through an air (oxygen) inlet 2, and SO is passed2SO is added into a gas inlet 32Gas, comprehensively adjusting each reaction parameter, and quickly dissolving copper to generate CuSO4When Cu is in solution2+Stopping the reaction when the concentration is 100g/L or more, and discharging the resultant solution through a dissolved solution discharge port of the copper dissolving tankThe produced qualified copper sulfate solution is discharged from a dissolving solution outlet 4, and the waste gas is discharged from an exhaust outlet 7.
The volume of the copper tank is determined according to production requirements, and is generally 3-120m3The height is 3-6m, the solid copper can be copper blocks, copper grains, copper wires, copper powder and the like, the stacking thickness of the solid copper is based on the smooth passing of mixed gas, and the copper dissolving tank can be designed with a plurality of solid copper discharging layers; the dissolving solution is a mixed solution prepared from sulfuric acid and copper sulfate, wherein the concentration of the sulfuric acid in the mixed solution is generally between 30 and 180g/L, and is optimally 80 to 90g/L, the acidity is maintained to be stable by replenishing at any time in the production process, and Cu is added2+The initial concentration is generally between 0 and 55g/L, preferably between 15 and 25g/L, the volume of the dissolving solution is determined according to production requirements, and if the volume is not enough, a dissolving solution tank can be independently arranged and is connected with a copper dissolving tank in series for use; if the requirement on the copper content of the copper dissolving liquid is high, a plurality of copper dissolving tanks can be connected in series for use, and the series stage number is determined according to the production requirement. Introducing compressed air into the solution from the bottom of the copper dissolving tank, wherein the air pressure is 0.03-0.3Mpa, and the flow is 5-550m3Between h, introducing SO into the compressed air before the compressed air enters the dissolving tank2Gas, SO2The gas pressure is 0.035-0.35, and the flow rate is 0.15-55 m3Between/h, compressed air and SO2The volume ratio of gas is 100: 3-10, introducing SO2。
Example 1
A method for quickly dissolving copper comprises the following steps:
(1) cutting cathode copper or waste copper into blocks of 100X 100mm, adding into a copper dissolving tank (phi 2500X 4000 mm), adding copper about 5 tons, and stacking to a thickness of about 1.0m, and sealing the feed inlet;
(2) starting a circulating pump, adding a dissolving solution into a copper dissolving tank, wherein the dissolving solution comprises sulfuric acid, water and a copper sulfate solution, the sulfuric acid concentration is about 85g/L, and the Cu concentration is about 85g/L2+The concentration is about 10g/L, and the volume of the solution is 15m3；
(3) Starting heating equipment, and heating the solution to 50-60 ℃;
(4) introducing compressed air into the copper dissolving tank, and compressingAir flow 100m3H, pressure: 0.25 MPa;
(5) introducing SO into compressed air2Flow 4.5m3H, pressure: 0.25 MPa;
(6) dissolving for about 5h, dissolving Cu in a copper dissolving tank2+The concentration reaches 100g/L, and the production requirement of the next procedure is met;
(7) and sending the qualified copper dissolving liquid to a downstream process for application.
Example 2
A method for quickly dissolving copper comprises the following steps:
(1) adding copper wires into a copper dissolving tank, wherein the diameter phi of the copper wires is 1mm, the length of the copper wires is 600mm, the phi of the copper dissolving tank is 2500 multiplied by 4000mm, the adding amount is about 5 tons, the material layer stacking thickness is about 1.5m, and then closing a feeding port;
(2) starting a circulating pump, adding a dissolving solution into a copper dissolving tank, wherein the dissolving solution comprises sulfuric acid, water and a copper sulfate solution, the sulfuric acid concentration is about 85g/L, and the Cu concentration is about 85g/L2+The concentration is about 10g/L, and the volume of the solution is 14.5m3Timely supplementing sulfuric acid when the concentration of sulfuric acid in the solution is lower than 20 g/L;
(3) starting heating equipment, heating the solution to 50-60 ℃, and then stopping heating;
(4) compressed air is introduced into the copper dissolving tank, and the flow rate of the compressed air is 120m3H, pressure: 0.25 MPa;
(5) introducing SO into compressed air2Flow rate of 5.0m3H, pressure: 0.25 MPa;
(6) dissolving for about 4h, dissolving Cu in a copper dissolving tank2+The concentration reaches 100g/L, and the production requirement of the next procedure is met;
(7) and sending the qualified copper dissolving liquid to a downstream process for application.
Example 3
A method for quickly dissolving copper comprises the following steps:
(1) adding copper powder into a copper dissolving tank, and adding powder D5070-100 upsilon m, phi 2500 x 4000mm of the copper dissolving tank, about 3.5 tons of adding amount, about 0.35m of stacking thickness of material layers and then sealing a feeding port;
（2）starting a circulating pump, adding a dissolving solution into a copper dissolving tank, wherein the dissolving solution comprises sulfuric acid, water and a copper sulfate solution, the sulfuric acid concentration is about 85g/L, and the Cu concentration is about 85g/L2+The concentration is about 10g/L, and the volume of the solution is 15.5m3Timely supplementing sulfuric acid when the concentration of sulfuric acid in the solution is lower than 20 g/L;
(3) starting heating equipment, heating the solution to 50-60 ℃, and then stopping heating;
(4) compressed air is introduced into the copper dissolving tank, and the flow rate of the compressed air is 125m3H, pressure: 0.25 MPa;
(5) introducing SO into compressed air2Flow rate of 5.0m3H, pressure: 0.25 MPa;
(6) dissolving for about 3.8h, dissolving Cu in a copper dissolving tank2+The concentration reaches 100g/L, and the production requirement of the next procedure is met;
(7) and sending the qualified copper dissolving liquid to a downstream process for application.
Claims (8)
1. A method for quickly dissolving copper is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
a. adding solid copper and a dissolving solution into a copper dissolving tank in sequence, wherein the dissolving solution is a mixed solution prepared from sulfuric acid and copper sulfate, the sulfuric acid concentration in the mixed solution is 80-90g/L, and the Cu concentration in the mixed solution is Cu2+The initial concentration is 15-25 g/L;
b. heating the solution to 50-65 deg.C, stopping heating, introducing 0.03-0.3Mpa compressed air into the solution from the bottom of copper dissolving tank at flow rate of 5-550m3H, introducing 0.035-0.35Mpa into the compressed air before the compressed air enters the dissolving tank, and the flow rate is 0.15-55 m3SO of/h2Gas, compressed air and SO2The volume ratio of the gas to the gas is 100: 3-10, increasing the oxidation potential of the solution, and quickly oxidizing the dissolved copper to generate CuSO4；
The addition amount of the dissolving solution is 2.9-4.5m per ton of solid copper3And (6) counting.
2. The method for rapid copper dissolution according to claim 1, wherein: the solid copper is any one of copper blocks, copper rice, copper wires and copper powder.
3. The method for rapid copper dissolution according to claim 2, wherein: SO introduced into the compressed air before it enters the dissolving tank2The pressure of the gas is higher than the pressure of the compressed air.
4. A method for rapid copper dissolution according to claim 3, wherein: the volume of the dissolving solution is determined according to production requirements, and when the volume is insufficient, the dissolving solution tank is separately arranged and is connected with the copper dissolving tank in series for use; when the copper content in the dissolving solution is high, a plurality of copper dissolving tanks are connected in series for use.
5. The method for rapid copper dissolution according to claim 1 or 4, wherein: compressed air and SO are introduced2The oxidation potential of the dissolved solution after the gas is increased from 500mV of 400 to 1200mV of 1000.
6. The method for rapid copper dissolution according to claim 5, wherein: cu in solution2+When the concentration exceeds or equals to 100g/L, the reaction is stopped and the reaction product is discharged through a dissolved solution discharge port of the copper dissolving tank.
7. A method of rapid copper dissolution according to claim 1, 2, 3, 4 or 6, wherein: the volume of the copper dissolving tank is 3-120m3And the height is 3-6 m.
8. The method for rapid copper dissolution according to claim 7, wherein: and a plurality of discharging layers for placing solid copper are arranged in the copper dissolving tank.
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| CN111850603B (en) * | 2020-07-08 | 2021-11-23 | 珠海格力绿色再生资源有限公司 | Recovery device and recovery method for oil-containing copper sludge |
| CN113457611B (en) * | 2021-07-06 | 2022-08-05 | 江西鑫铂瑞科技有限公司 | Electrolytic copper foil copper dissolving material process capable of reducing energy consumption |
| CN115108592A (en) * | 2022-06-30 | 2022-09-27 | 金川集团股份有限公司 | Production method of high-purity cobalt sulfate |
| CN115178164A (en) * | 2022-07-05 | 2022-10-14 | 西安航天源动力工程有限公司 | Preparation device and preparation method of copper sulfate electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1335264A (en) * | 2001-09-03 | 2002-02-13 | 贾荣宝 | Wet low-temperature oxidation and decomposition process of producing active copper oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1335264A (en) * | 2001-09-03 | 2002-02-13 | 贾荣宝 | Wet low-temperature oxidation and decomposition process of producing active copper oxide |
Non-Patent Citations (1)
| Title |
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| "大气中SO2对铜的腐蚀行为研究";葛红花等;《上海电力学院学报》;20101231;第26卷(第06期);摘要部分，第577页第1段，第579页第3-5段以图3，第580页第1-6段 * |
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