CN104313653A - Method for preparing electrolyte for copper foil electrolysis by using regenerated copper oxide - Google Patents
Method for preparing electrolyte for copper foil electrolysis by using regenerated copper oxide Download PDFInfo
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- CN104313653A CN104313653A CN201410485956.5A CN201410485956A CN104313653A CN 104313653 A CN104313653 A CN 104313653A CN 201410485956 A CN201410485956 A CN 201410485956A CN 104313653 A CN104313653 A CN 104313653A
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- copper
- electrolyte
- copper foil
- electrolytic
- regenerating oxidation
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Abstract
The invention discloses a method for preparing an electrolyte for copper foil electrolysis by using regenerated copper oxide, and belongs to the technical field of the preparation process of electrolyte. The main technical points comprise the following steps: (1) adding sulfuric acid electrolyte into a copper pot and heating; (2) when the temperature rises to 55 to 65 DEG C, adding powdery regenerated copper oxide; (3) after addition of the regenerated copper oxide, stirring for dissolution reaction for 25-35 minutes; (4) if the reaction solution is tested to be clarified and have standard reached copper content, adding powder activated carbon into the copper pot and ventilating for cleaning treatment for 25-35 minutes; and (5) after cleaning adsorption, filtering the activated carbon to obtain the copper sulfate electrolyte for copper foil electrolysis. The invention aims to provide a method for preparing the electrolyte for copper foil electrolysis by using regenerated copper oxide at low production cost and stable quality, and the method can be used for preparing electrolyte for copper foil electrolysis.
Description
Technical field
The present invention relates to a kind of preparation method of electrolytic copper foil electrolytic solution, more particularly, particularly relate to a kind of regenerating oxidation copper that uses for the method for electrolytic copper foil electrolytic solution.
Background technology
Electrolytic copper foil carries out electroplating deposition acquisition by using cathode roller and positive plate to copper sulfate electrolyte, so copper sulfate electrolyte component target is most important in electrolytic copper foil production process, and the cupric ion index (Cu particularly in sulfuric acid electrolyte
2+), because electrolytic copper foil production process constantly deposits copper from electrolytic solution, just need to supplementation with copper ion in electrolytic solution to maintain the balance of electrolytic solution index, so the control of cupric ion is that electrolytic copper foil production process is difficult to control in electrolytic solution.In conventional electrolysis Copper Foil production process, in electrolytic solution, the supplementary of cupric ion is by using the low copper containing amount electrolyte stream of system pipeline and storage tank through storing the tank body of copper cash or copper coin, to obtain the electrolytic solution of rich copper content, this tank body is referred to as copper dissolving tank, copper cash or copper coin are a kind of processes of oxidation dissolution in this copper dissolving tank, because the dissolution process of copper can be subject to solvent temperature, with sour contact area, the impact of the factors such as copper material periphery electrolytic solution saturation ratio, so, often occur copper material stack better time or envrionment temperature higher time copper dissolving tank in good to the dissolving power of copper material, otherwise then dissolving power is poor, site operation personnel is difficult to observe and recognize the copper material situation in copper dissolving tank, so the cupric ion in electrolyte system belongs to fluctuation status, analyze from production cost aspect, owing to having enough copper materials and electrolyte contacts area in copper dissolving tank to ensure, a large amount of copper materials must be laid in copper dissolving tank, the cost of fund producing material will inevitably be increased thus.
The cupric oxide used in method of the present invention reclaims for utilizing copper-clad plate manufacturer etching solution making of purifying, belong to the environmental friendly regenerated utilization of resources, there is long-range environmental protection value of exploiting and utilizing, this type of cupric oxide is due to the impact of production technique, its purity is generally about 80%, and other 20% composition is mainly water and organic impurity, because the raw materials for production of above-mentioned cupric oxide come as various copper-clad plate factory, generally various organic additive can be added in etching solution in each copper-clad plate factory, to reach needed for copper-clad plate production, therefore these type of cupric oxide starting material are compared the cupric oxide that dry method cures out and can be contained more organic impurity.
Summary of the invention
The object of the invention is to for above-mentioned the deficiencies in the prior art, provide a kind of production cost low, stay-in-grade use regenerating oxidation copper for the method for electrolytic copper foil electrolytic solution.
Technical scheme of the present invention is achieved in that a kind of regenerating oxidation copper that uses is for the method for electrolytic copper foil electrolytic solution, comprises the steps: that (1) adds sulfuric acid electrolyte in copper dissolving tank, heats simultaneously to sulfuric acid electrolyte; (2) when temperature is increased to 55-65 DEG C, add the regenerating oxidation copper of powdery, the proportionlity between the addition of regenerating oxidation copper and sulfuric acid electrolyte is every 1m
3sulfuric acid electrolyte adds 0.06-0.08t regenerating oxidation copper; (3), after regenerating oxidation copper has added, stir and carry out solubilizing reaction, the reaction times is 25-35 minute; (4) the solution clarification after detection reaction and copper content up to standard time, toward copper dissolving tank in, add powdered active carbon and Ex-all process is carried out in ventilation, the proportionlity in gac and copper dissolving tank between solution is every 1m
3solution adds 0.6-1kg gac, and stir and carry out Ex-all absorption, the time is 25-35 minute; (5), after Ex-all has been adsorbed, filter out gac and obtain electrolytic copper foil copper sulfate electrolyte.
Above-mentioned a kind ofly use in the method for regenerating oxidation copper for electrolytic copper foil electrolytic solution, in step (2), the interpolation speed of regenerating oxidation copper is 0.07-0.1t/min.
Above-mentioned a kind ofly use in the method for regenerating oxidation copper for electrolytic copper foil electrolytic solution, the stirring velocity that solubilizing reaction is carried out in step (3) described stirring is 100-150r/min.
Above-mentioned a kind ofly use in the method for regenerating oxidation copper for electrolytic copper foil electrolytic solution, in step (4) add powdered active carbon granularity be 20-50 order, the order number of described gac is 200-500 order.
After the present invention adopts aforesaid method, the cupric ion of application electrolytic copper foil production process electrolytic solution supplements, and its corresponding production process is molten copper (or liquid processed) operation, compared with prior art, has following advantage:
(1) make electrolytic copper foil in production process, the content of copper ion of its electrolytic solution obtains stable control, to make supplementing of cupric ion in molten copper (or liquid processed) operation can quantum chemical method;
(2) by using this method, improve efficiency prepared by electrolytic solution in electrolytic copper foil production process, reducing the energy consumption in production process, decrease the deposit of the high copper material of price, and then reach reduction production cost.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but do not form any limitation of the invention.
A kind of regenerating oxidation copper that uses of the present invention, for the method for electrolytic copper foil electrolytic solution, comprises the steps:
(1) in copper dissolving tank, add sulfuric acid electrolyte, sulfuric acid electrolyte is heated simultaneously.
(2) when temperature is increased to 55-65 DEG C, add the regenerating oxidation copper of powdery, the proportionlity between the addition of regenerating oxidation copper and sulfuric acid electrolyte is every 1m
3sulfuric acid electrolyte adds 0.06-0.08t regenerating oxidation copper; The interpolation speed of regenerating oxidation copper is 0.07-0.1t/min.The regenerating oxidation copper used in the inventive method, reclaim to purify for utilizing copper-clad plate manufacturer etching solution and make, belong to the environmental friendly regenerated utilization of resources, there is long-range environmental protection value of exploiting and utilizing, this type of cupric oxide is due to the impact of production technique, its purity is generally about 80%, and other 20% composition is mainly water and organic impurity, because the raw materials for production of above-mentioned cupric oxide come as various copper-clad plate factory, generally various organic additive can be added in etching solution in each copper-clad plate factory, to reach needed for copper-clad plate production, therefore these type of cupric oxide starting material are compared the cupric oxide that dry method cures out and can be contained more organic impurity.
(3), after regenerating oxidation copper has added, stir and carry out solubilizing reaction, stirring velocity is 100-150r/min, and the reaction times is 25-35 minute.
(4) after detection reaction solution clarification and copper content up to standard time, when copper content finger copper up to standard content is 120-140g/l, in copper dissolving tank, add powdered active carbon and ventilate and carry out Ex-all process, the proportionlity in gac and copper dissolving tank between solution is every 1m
3solution adds 0.6-1kg gac, and stir and carry out Ex-all absorption, the time is 25-35 minute; The granularity of powdered active carbon described in the present embodiment is 20-50 order, and the order number of described gac is 200-500 order.
(5), after Ex-all has been adsorbed, filter out gac and obtain electrolytic copper foil copper sulfate electrolyte.
Implement principle:
The principle that copper cash or copper coin dissolved in copper dissolving tank is in the past:
2CuO+O
2+H
2SO
4＝2CuSO
4+2H
2O
Visible, in copper cash or copper coin dissolution process, need to pass into a large amount of air to make copper cash or copper coin rapid oxidation, then carry out reaction with sulfuric acid and generate copper sulfate; The acquisition of large quantity of air is undertaken by blast apparatus, the electric energy that this process need consumption is a large amount of.
And when using regenerative ratio cupric oxide to prepare electrolytic solution, its reaction principle is:
CuO+H
2SO
4＝CuSO
4+H
2O
Can be found out by above-mentioned reaction formula, cupric oxide and sulfuric acid can direct reaction, do not need to pass into air, thus save a large amount of electric energy, and owing to reducing reaction process required air factor, make the solubilizing reaction of cupric oxide very fast, so can easily calculate dissolved content of copper ion.
But owing to being the feature of spent solution regeneration cupric oxide, containing other a large amount of organic impuritys in this type of regenerative ratio cupric oxide, in the checking by electrolytic copper foil production process, find that electrolytic solution prepared by this type of cupric oxide is very big to Influence of production, easily cause the generation of the different shape problem of copper foil surface, so, the inventive method utilize principle for: the process of organics removal must be carried out to dissolved electrolytic solution when using this type of cupric oxide, proved by production practice, after use gac carries out circulating filtration process to prepared electrolytic solution, to electrolytic copper foil produce be do not have influential.
Experimental example:
Major equipment: copper dissolving tank, strainer, pump, well heater, roots blower
Main raw: regenerating oxidation copper: CuO content 80%, moisture content and in fact foreign matter content 20%
Filtering requirement: 10 micron filter bag
Gac proportional quantity: gac is 200 order Powdered Activated Carbons, and granularity is less than 20 orders, activated carbon dosage ratio: gac compares 0.8kg:1m with electrolytic solution
3.
Three, operating process:
Copper oxide dissolves operating process:
1, completed by copper dissolving tank.
2, before dissolving adds cupric oxide, check copper dissolving tank, to ensure in tank without copper cash, gac, the paper tinsel that gives up, split pipe air-supply duct without blocking, tank body is clean.
3, copper dissolving tank and filter pipeline inspection: each valve closes, exhaust-valve is closed, each flange bolt fastening one time.
4, after valve transfer inspection normally, open copper dissolving tank liquid flowing valve, air feed valve open, hot-water valve is opened and is started heating unit into water standard-sized sheet simultaneously.
5,40m is used
3sulfuric acid electrolyte enters to dissolve, and sulfuric acid electrolyte and regenerating oxidation copper ratio are 40m
3: 2.8t, when copper dissolving tank liquid measure is 40m
3time valve-off.
6, when copper dissolving tank electrolyte temperature is to 60 degree, start to add cupric oxide, the shape that must fall apart when adding cupric oxide adds, and drop into after must breaing up if any conglomeration, 2.8t regenerating oxidation copper controls evenly slowly to add at 30-40 minute again.
7, regenerating oxidation copper has added to dissolve for rear etc. 30 minutes and has stirred, then gets electrolytic solution filter paper filtering and check that electrolytic solution is for clarification, checks once until clarification every 10 points when not clarifying again.It is 130g/l that copper content is done in sampling.
8, after electrolytic solution clarification, in copper dissolving tank, add Powdered Activated Carbon carry out Ex-all process, proportion requirement is: gac compares 0.8kg:1m with electrolytic solution
3, (namely gac is 32kg), now air feed stirs and does not still stop, with gac Ex-all 30 minutes.
9, add after gac circulates 30 minutes, open valve, start internal recycling pump and filtration cycle is carried out to electrolytic solution.
10, valve transfer good after start noncorrosive pump immediately, note filter pressure, feed flow valve is opened when pressure reaches 0.1Mpa, the copper-bath of generation is supplied to production line, open required uninterrupted according to production of copper content requirement, now can go out flow quantity by detection feed flow valve export, to calculate on production line content of copper ion in replenishment system, by to the deposition quantitative analysis of producing board, to adjust suitable valve flow.
11, produce when feed flow valve wide open when flow does not reach the requirement of supplementation with copper ion or filter pressure is greater than 0.3Mpa, stop acid proof pump and change filter bag.(change filter bag for repeating operation, once, then with the content of step 10 again operation start noncorrosive pump, filter bag cleaning is leaked filter can use again without damaged in replacing about per hour.)
12, change filter bag time must ensure can not because of filter bag break and fit sealing cause Lous filter.Noncorrosive pump and pipeline crystallization can not be caused because shutting down when changing filter cloth bag.
13, as copper dissolving tank 40m
3after electrolytic solution is found time, after stopping noncorrosive pump, replacing filter bag carried out to strainer and rinses pump housing pipeline, preventing crystallization.Again again by this operation tapping dissolved oxygen copper operation, copper ion concentration requirement needed for raw paper tinsel is ensured.
Claims (4)
1. use regenerating oxidation copper for a method for electrolytic copper foil electrolytic solution, it is characterized in that, comprise the steps: that (1) adds sulfuric acid electrolyte in copper dissolving tank, sulfuric acid electrolyte is heated simultaneously; (2) when temperature is increased to 55-65 DEG C, add the regenerating oxidation copper of powdery, the proportionlity between the addition of regenerating oxidation copper and sulfuric acid electrolyte is every 1m
3sulfuric acid electrolyte adds 0.06-0.08t regenerating oxidation copper; (3), after regenerating oxidation copper has added, stir and carry out solubilizing reaction, the reaction times is 25-35 minute; (4) the solution clarification after detection reaction and copper content up to standard time, toward copper dissolving tank in, add powdered active carbon and Ex-all process is carried out in ventilation, the proportionlity in gac and copper dissolving tank between solution is every 1m
3solution adds 0.6-1kg gac, and stir and carry out Ex-all absorption, the time is 25-35 minute; (5), after Ex-all has been adsorbed, filter out gac and obtain electrolytic copper foil copper sulfate electrolyte.
2. a kind of regenerating oxidation copper that uses according to claim 1 is for the method for electrolytic copper foil electrolytic solution, it is characterized in that, in step (2), the interpolation speed of regenerating oxidation copper is 0.07-0.1t/min.
3. a kind of regenerating oxidation copper that uses according to claim 1 is for the method for electrolytic copper foil electrolytic solution, it is characterized in that, the stirring velocity that solubilizing reaction is carried out in step (3) described stirring is 100-150r/min.
4. a kind of regenerating oxidation copper that uses according to claim 1 is for the method for electrolytic copper foil electrolytic solution, it is characterized in that, in step (4) add powdered active carbon granularity be 20-50 order, the order number of described gac is 200-500 order.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113481547A (en) * | 2021-07-05 | 2021-10-08 | 江西鑫铂瑞科技有限公司 | Method for using raw material water quenched copper for electrolytic copper foil production |
| CN114990642A (en) * | 2022-06-15 | 2022-09-02 | 云南润久科技有限公司 | Electrolyte rapid liquid making method and circulating system in electrolytic copper foil production |
| CN116180166A (en) * | 2023-03-01 | 2023-05-30 | 安徽华创新材料股份有限公司 | Production method of 3.5-4 mu m double-sided light copper foil |
| CN116180166B (en) * | 2023-03-01 | 2024-05-03 | 安徽华创新材料股份有限公司 | Production method of 3.5-4 mu m double-sided light copper foil |
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| CN116180166B (en) * | 2023-03-01 | 2024-05-03 | 安徽华创新材料股份有限公司 | Production method of 3.5-4 mu m double-sided light copper foil |
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