CN105483743A - Device and method for preparing cuprous oxide through electrolysis - Google Patents
Device and method for preparing cuprous oxide through electrolysis Download PDFInfo
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- CN105483743A CN105483743A CN201410472519.XA CN201410472519A CN105483743A CN 105483743 A CN105483743 A CN 105483743A CN 201410472519 A CN201410472519 A CN 201410472519A CN 105483743 A CN105483743 A CN 105483743A
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Abstract
The invention discloses a device and method for preparing cuprous oxide through electrolysis. The device for preparing the cuprous oxide through electrolysis comprises an electrolytic cell containing alkaline electrolyte, an electrolytic copper piece serving as the anode and an impure-red-copper plate serving as the cathode, wherein the electrolytic copper piece and the impure-red-copper plate are inserted into the electrolytic cell in a spaced mode and connected with the positive pole and the negative pole of a power source respectively. According to the device and method for preparing the cuprous oxide through electrolysis, the process is simple, and operation is convenient; a sodium chromate solution is used as an additive, the content of metallic copper in a product is effectively lowered, and the purity of the obtained cuprous oxide is high and can reach more than 95%.
Description
Technical field
The present invention relates to the preparation technology of Red copper oxide, be specifically related to the apparatus and method that a kind of electrolytic process prepares Red copper oxide.
Background technology
Red copper oxide is a kind of important Inorganic Chemicals, and in anti-fouling ship paint, red glass, enamel pigment, electric ballast material, agricultural chemicals etc., tool has been widely used.The preparation method of Red copper oxide mainly contains electrolytic process, sintering process, sulphite or method of glucose reduction etc.Sintering process is with electrolytic copper powder and cupric oxide powder for raw material high-temperature calcination, and energy consumption is huge, and three-waste pollution is serious, and is not easy the Red copper oxide that obtained purity is high, particle is little; Although sulphite or method of glucose reduction can obtain the very high product of purity, a large amount of consumption of chemical reagent and should not large-scale production make it be difficult to promote.By contrast, electrolytic process has that technical process is simple, energy consumption is low, output is high, processing ease, is suitable for the advantages such as suitability for industrialized production, has good industrial prospect.
Summary of the invention
The object of the invention is to provide the apparatus and method that a kind of electrolytic process prepares Red copper oxide, and technique is simple, easy to operate, and obtained Red copper oxide purity is high.
For achieving the above object, the technical solution used in the present invention is: a kind of electrolytic process prepares the device of Red copper oxide, comprise the electrolyzer, the electrolytic copper foil as anode and the recycled copper plate as negative electrode that fill alkaline electrolyte, described electrolytic copper foil and recycled copper plate interval are inserted in electrolyzer, and described electrolytic copper foil, recycled copper plate are connected with the positive and negative electrode of power supply respectively.
In technique scheme, in the electrolytic solution of described electrolyzer, be fitted with recycled copper plate described in electrolytic copper foil described in two and three, and all electrolytic copper foil and recycled copper plate keep contraposition consistent to line, interpole gap.
Further technical scheme, described electrolytic solution is exposed in the upper end of described electrolytic copper foil, and is connected with positive source by an anode copper rod be connected with it;
Described electrolytic solution is exposed in the upper end of described recycled copper plate, and is connected with power cathode by a negative electrode copper rod be connected with it.
Preferably, described electrolyzer is stainless steel tank, and its inwall is provided with liner glue-line.
In technique scheme, the outside of described electrolyzer is provided with steam insulation device.
The embodiment of the present invention also provides a kind of method utilizing the electrolytic process of said apparatus to prepare Red copper oxide, comprises the steps:
(1) two pieces of electrolytic copper foil and three blocks of recycled copper plates are inserted in electrolyzer, and keep contraposition consistent to line, interpole gap;
(2) by proportion be 1.185 ~ 1.2 sodium chloride solution heat in reactor, simultaneously in sodium chloride solution, add sodium hydroxide solution, make its pH value be 10 ~ 12, temperature is 95 ~ 100 DEG C;
(3) electrolytic solution after heating in step (2) is poured in electrolyzer, add chromium acid sodium solution simultaneously and make additive, until 5 ~ 8cm below liquid level to cathode and anode upper end, open steam insulation device, utilize steam insulation;
(4) opening power, starts electrolysis, and at normal electrolysis time control electric current 130 ~ 160A; Voltage 36 ~ 40V, per hourly adds chromium acid sodium solution 50ml, adds 1:1 hydrochloric acid 250ml per half an hour;
(5) the once electrolytic time is 50 ~ 60 hours, and the add-on of record temperature per hour, pH value, electric current, voltage and Sodium chromate once;
(6) after electrolysis terminates, cut off the electricity supply, the material in electrolyzer is released one by one, hang out all electrolytic copper foil and recycled copper plate simultaneously;
(7) with the inwall of appropriate water cleaning electrolyzer and valve;
(8) clean yin, yang pole plate: by yin, yang pole plate and on copper rod put into cleaning cylinder carefully, add water to the yin, yang pole plate that submergence is all, be added to the 0.5h that boils, rinse to redgreen in electrolytic copper foil and recycled copper plate with clear water after taking out in self-stip cylinder;
(9) the cuprous oxide powder steam boiling being deposited in cell bottom during electrolysis is screened in suction filtration cylinder to during near doing with 100 eye mesh screens, once wash with the deionized water that temperature is 80 DEG C, acidifying is carried out again with the sulfuric acid that concentration is 15g/L, then be washed till sulfate radical-free with the deionization intermediate water that temperature is 80 DEG C and carry out suction filtration, be 80kPa by Red copper oxide good for suction filtration to vacuum tightness, temperature is dry in the vacuum drying oven of 100 DEG C-105 DEG C, go out when being dried to moisture content≤0.5% to be delivered to after amalgamator mixes and stirs half an hour after baking oven is cooled to normal temperature and pack, the Red copper oxide of obtained finished product.
Wherein, described step (1) electrolytic copper foil insertion electrolyzer before, to its perforating, shearing, cleaning, installation hanger, affixed copper rod.
Wherein, the massfraction of sodium hydroxide solution used in described step (2) is 20%.
Wherein, in described step (3) and (4), the massfraction of chromium acid sodium solution used is 10%.
Wherein, in described step (3), add the chromium acid sodium solution of 200ml, massfraction 10% in every groove, in described step (5), the output of once electrolytic is about 1.5 ~ 2.
Wherein, in described step (9), during boiling cuprous oxide powder, need oxygenant be added, during secondary washing, in water, add preservation agent;
Boiling temperature is 100 DEG C;
Souring temperature is 70 DEG C, liquid-solid ratio 2:1.
Wherein, in described step (9) once washing and secondary wash after waste water first enter in pond for recovering, treated rear discharge up to standard.
Because technique scheme is used, the present invention compared with prior art has following advantages:
The apparatus and method technique that electrolytic process provided by the invention prepares Red copper oxide is simple, easy to operate, take chromium acid sodium solution as additive, and effectively reduce the content of metallic copper in product, obtained Red copper oxide purity is high, can reach more than 95%.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the present invention one.
Description of reference numerals:
1, electrolyzer;
2, electrolytic copper foil; 20, anode copper rod;
3, recycled copper plate; 30, negative electrode copper rod;
4, steam insulation device.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
Shown in embodiment one: Fig. 1, a kind of electrolytic process prepares the device of Red copper oxide, and comprise the electrolyzer 1, the electrolytic copper foil 2 as anode and the recycled copper plate 3 as negative electrode that fill alkaline electrolyte, described electrolyzer 1 is stainless steel tank, and its inwall is provided with liner glue-line.
Described electrolytic copper foil 2 and recycled copper plate 3 interval are inserted in electrolyzer 1, and described electrolytic copper foil 2, recycled copper plate 3 are connected with the positive and negative electrode of power supply respectively.
In the present embodiment, be fitted with two pieces of described electrolytic copper foil 2 and three blocks of described recycled copper plates 3 in the electrolytic solution of described electrolyzer 1, and all electrolytic copper foil 2 and recycled copper plate 3 keep contraposition consistent to line, interpole gap.
Described electrolytic solution is exposed in the upper end of described electrolytic copper foil 2, and is connected with positive source by an anode copper rod 20 be connected with it.
Described electrolytic solution is exposed in the upper end of described recycled copper plate 3, and is connected with power cathode by a negative electrode copper rod 30 be connected with it.
The outside of described electrolyzer 1 is provided with steam insulation device 4.
The embodiment of the present invention one also provides a kind of method utilizing the electrolytic process of said apparatus to prepare Red copper oxide, comprises the steps:
(1) two pieces of electrolytic copper foil and three blocks of recycled copper plates are inserted in electrolyzer, and keep contraposition consistent to line, interpole gap;
Wherein, electrolytic copper foil, need to its perforating, shearing, cleaning, installation hanger, affixed copper rod before insertion electrolyzer.
(2) by proportion be 1.185 ~ 1.2 sodium chloride solution heat in reactor, simultaneously in sodium chloride solution, add the sodium hydroxide solution that massfraction is 20%, make its pH value be 10 ~ 12, temperature is 95 ~ 100 DEG C;
(3) electrolytic solution after heating in step (2) is poured in electrolyzer, simultaneously add 200ml in every groove, massfraction be 10% chromium acid sodium solution make additive, until 5cm below liquid level to cathode and anode upper end, open steam insulation device, utilize steam insulation;
(4) opening power, starts electrolysis, and at normal electrolysis time control electric current 130 ~ 160A; Voltage 36 ~ 40V, per hourly adds the chromium acid sodium solution 50ml that massfraction is 10%, adds 1:1 hydrochloric acid 250ml per half an hour;
(5) the once electrolytic time is 50 ~ 60 hours, and output is about 1.5 ~ 2, and the add-on of record temperature per hour, pH value, electric current, voltage and Sodium chromate once;
(6) after electrolysis terminates, cut off the electricity supply, the material in electrolyzer is released one by one, hang out all electrolytic copper foil and recycled copper plate simultaneously;
(7) with the inwall of appropriate water cleaning electrolyzer and valve;
(8) clean yin, yang pole plate: by yin, yang pole plate and on copper rod put into cleaning cylinder carefully, add water to the yin, yang pole plate that submergence is all, be added to the 0.5h that boils, rinse to redgreen in electrolytic copper foil and recycled copper plate with clear water after taking out in self-stip cylinder;
(9) the cuprous oxide powder steam boiling (boiling temperature is 100 DEG C) being deposited in cell bottom during electrolysis is screened in suction filtration cylinder to during near doing with 100 eye mesh screens, once wash with the deionized water that temperature is 80 DEG C, (souring temperature is 70 DEG C to carry out acidifying with the sulfuric acid that concentration is 15g/L again, liquid-solid ratio 2:1), then be washed till sulfate radical-free with the deionization intermediate water that temperature is 80 DEG C and carry out suction filtration, be 80kPa by Red copper oxide good for suction filtration to vacuum tightness, temperature is dry in the vacuum drying oven of 100 DEG C-105 DEG C, go out when being dried to moisture content≤0.5% to be delivered to after amalgamator mixes and stirs half an hour after baking oven is cooled to normal temperature and pack, the Red copper oxide of obtained finished product,
Wherein, during boiling cuprous oxide powder, need oxygenant be added, during secondary washing, in water, add preservation agent; Once washing and secondary wash after waste water first enter in pond for recovering, treated rear discharge up to standard.
The apparatus and method technique that electrolytic process provided by the invention prepares Red copper oxide is simple, easy to operate, take chromium acid sodium solution as additive, and effectively reduce the content of metallic copper in product, obtained Red copper oxide purity is high, can reach more than 95%.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from principle of the present invention; can also make some improvement or replacement, these improve or replace and also should be considered as protection scope of the present invention.
Claims (11)
1. an electrolytic process prepares the device of Red copper oxide, it is characterized in that, comprise the electrolyzer, the electrolytic copper foil as anode and the recycled copper plate as negative electrode that fill alkaline electrolyte, described electrolytic copper foil and recycled copper plate interval are inserted in electrolyzer, and described electrolytic copper foil, recycled copper plate are connected with the positive and negative electrode of power supply respectively.
2. electrolytic process according to claim 1 prepares the device of Red copper oxide, it is characterized in that, be fitted with recycled copper plate described in electrolytic copper foil described in two and three in the electrolytic solution of described electrolyzer, and all electrolytic copper foil and recycled copper plate keep contraposition consistent to line, interpole gap.
3. electrolytic process according to claim 1 and 2 prepares the device of Red copper oxide, it is characterized in that, described electrolytic solution is exposed in the upper end of described electrolytic copper foil, and is connected with positive source by an anode copper rod be connected with it;
Described electrolytic solution is exposed in the upper end of described recycled copper plate, and is connected with power cathode by a negative electrode copper rod be connected with it.
4. electrolytic process according to claim 1 prepares the device of Red copper oxide, it is characterized in that, described electrolyzer is stainless steel tank, and its inwall is provided with liner glue-line.
5. the electrolytic process according to any one of claim 1,2 or 3 prepares the device of Red copper oxide, it is characterized in that, the outside of described electrolyzer is provided with steam insulation device.
6. utilize the electrolytic process of said apparatus to prepare a method for Red copper oxide, it is characterized in that, comprise the steps:
(1) two pieces of electrolytic copper foil and three blocks of recycled copper plates are inserted in electrolyzer, and keep contraposition consistent to line, interpole gap;
(2) by proportion be 1.185 ~ 1.2 sodium chloride solution heat in reactor, simultaneously in sodium chloride solution, add sodium hydroxide solution, make its pH value be 10 ~ 12, temperature is 95 ~ 100 DEG C;
(3) electrolytic solution after heating in step (2) is poured in electrolyzer, add chromium acid sodium solution simultaneously and make additive, until 5 ~ 8cm below liquid level to cathode and anode upper end, open steam insulation device, utilize steam insulation;
(4) opening power, starts electrolysis, and at normal electrolysis time control electric current 130 ~ 160A; Voltage 36 ~ 40V, per hourly adds chromium acid sodium solution 50ml, adds 1:1 hydrochloric acid 250ml per half an hour;
(5) the once electrolytic time is 50 ~ 60 hours, and the add-on of record temperature per hour, pH value, electric current, voltage and Sodium chromate once;
(6) after electrolysis terminates, cut off the electricity supply, the material in electrolyzer is released one by one, hang out all electrolytic copper foil and recycled copper plate simultaneously;
(7) with the inwall of appropriate water cleaning electrolyzer and valve;
(8) clean yin, yang pole plate: by yin, yang pole plate and on copper rod put into cleaning cylinder carefully, add water to the yin, yang pole plate that submergence is all, be added to the 0.5h that boils, rinse to redgreen in electrolytic copper foil and recycled copper plate with clear water after taking out in self-stip cylinder;
(9) the cuprous oxide powder steam boiling being deposited in cell bottom during electrolysis is screened in suction filtration cylinder to during near doing with 100 eye mesh screens, once wash with the deionized water that temperature is 80 DEG C, acidifying is carried out again with the sulfuric acid that concentration is 15g/L, then be washed till sulfate radical-free with the deionization intermediate water that temperature is 80 DEG C and carry out suction filtration, be 80kPa by Red copper oxide good for suction filtration to vacuum tightness, temperature is dry in the vacuum drying oven of 100 DEG C-105 DEG C, go out when being dried to moisture content≤0.5% to be delivered to after amalgamator mixes and stirs half an hour after baking oven is cooled to normal temperature and pack, obtained finished product Red copper oxide.
7. electrolytic process according to claim 5 prepares the method for Red copper oxide, it is characterized in that, the massfraction of sodium hydroxide solution used in described step (2) is 20%.
8. electrolytic process according to claim 5 prepares the method for Red copper oxide, it is characterized in that, in described step (3) and (4), the massfraction of chromium acid sodium solution used is 10%.
9. electrolytic process according to claim 5 prepares the method for Red copper oxide, it is characterized in that, in described step (3), add the chromium acid sodium solution of 200ml, massfraction 10% in every groove, in described step (5), the output of once electrolytic is about 1.5 ~ 2 tons.
10. electrolytic process according to claim 5 prepares the method for Red copper oxide, it is characterized in that, need add oxygenant in described step (9) during boiling cuprous oxide powder, adds preservation agent during secondary washing in water;
Boiling temperature is 100 DEG C;
Souring temperature is 70 DEG C, liquid-solid ratio 2:1.
11. electrolytic process according to claim 5 prepare the method for Red copper oxide, it is characterized in that, in described step (9) once washing and secondary wash after waste water first enter in pond for recovering, treated rear discharge up to standard.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410472519.XA CN105483743A (en) | 2014-09-16 | 2014-09-16 | Device and method for preparing cuprous oxide through electrolysis |
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| CN201410472519.XA CN105483743A (en) | 2014-09-16 | 2014-09-16 | Device and method for preparing cuprous oxide through electrolysis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107326382A (en) * | 2017-06-15 | 2017-11-07 | 江苏泰禾金属工业有限公司 | A kind of method of electrolytic preparation cuprous oxide powder under the conditions of low-temperature environment-friendly |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5325296A (en) * | 1976-08-20 | 1978-03-08 | Mitsubishi Metal Corp | Production of copper suboxide powder for pigment |
| CN1434151A (en) * | 2003-02-27 | 2003-08-06 | 华中师范大学 | Method for preparing nano copper protoxide material by metal copper anodic oxidation method |
| CN1556250A (en) * | 2003-12-31 | 2004-12-22 | �Ϻ���ͨ��ѧ | Electrolysis preparation method of nano cuprous oxide |
| CN1807688A (en) * | 2005-12-20 | 2006-07-26 | 厦门大学 | Process for preparing shape controllable cuprous oxide micro/nano crystal by electrochemical deposition |
-
2014
- 2014-09-16 CN CN201410472519.XA patent/CN105483743A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5325296A (en) * | 1976-08-20 | 1978-03-08 | Mitsubishi Metal Corp | Production of copper suboxide powder for pigment |
| CN1434151A (en) * | 2003-02-27 | 2003-08-06 | 华中师范大学 | Method for preparing nano copper protoxide material by metal copper anodic oxidation method |
| CN1556250A (en) * | 2003-12-31 | 2004-12-22 | �Ϻ���ͨ��ѧ | Electrolysis preparation method of nano cuprous oxide |
| CN1807688A (en) * | 2005-12-20 | 2006-07-26 | 厦门大学 | Process for preparing shape controllable cuprous oxide micro/nano crystal by electrochemical deposition |
Non-Patent Citations (2)
| Title |
|---|
| 刘铁军: ""电解法生产氧化亚铜粉末的工艺改进"", 《山东化工》 * |
| 天津化工研究院等: "《无机盐工业手册 下册》", 30 June 1992 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107326382A (en) * | 2017-06-15 | 2017-11-07 | 江苏泰禾金属工业有限公司 | A kind of method of electrolytic preparation cuprous oxide powder under the conditions of low-temperature environment-friendly |
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Application publication date: 20160413 |