CN103232056A - Method of preparing copper oxide - Google Patents
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- CN103232056A CN103232056A CN2013101233216A CN201310123321A CN103232056A CN 103232056 A CN103232056 A CN 103232056A CN 2013101233216 A CN2013101233216 A CN 2013101233216A CN 201310123321 A CN201310123321 A CN 201310123321A CN 103232056 A CN103232056 A CN 103232056A
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Abstract
The present invention provides a method of preparing copper oxide, comprising the steps of: preparing a Cu<2+> containing acidic solution, a CO3<2-> and OH<-> containing solution and a CH3COO<-> containing solution as a liquid C for use; injecting the above solutions into a reactor for a primary reaction, after the primary reaction is completed, adding an OH<-> containing solution in the reactor, heating for reactions, and performing washing and preliminary dehydration treatments to an obtained product to obtain a preliminary product after the reaction is completed; and performing a dehydration treatment to the preliminary product, drying at a temperature of 50 DEG C -150 DEG C to obtain the target product copper oxide. According to the invention, copper chloride and copper sulfate are used as starting materials, wherein the copper chloride can be obtained through treatment of waste copper circuits or direct use of circuit board copper chloride waste fluid, and the copper sulfate can be obtained through reextraction by using sulfuric acid after extraction of copper ores or waste copper materials; so the starting materials of the method have relatively low prices, and the use of cheap, readily available and non-toxic starting materials improves production efficiency and product quality, and reduces production costs of the copper oxide.
Description
Technical field
The present invention relates to chemical production field, relate in particular to a kind of preparation method of cupric oxide.
Background technology
Cupric oxide of many uses, main preparation methods is dry method and wet method at present.Mainly by the wet processing preparation, the purposes of active copper oxide is also more extensive for active copper oxide.But present a lot of wet method preparation process is thin because of the product granularity of cupric oxide, causes the impurity for preparing after finishing not utilize and washes, thereby influences the purity of product.Want thorough purged of impurities to obtain highly purified active copper oxide, need a large amount of rinse water and washing repeatedly, can increase production cost like this and have a strong impact on production efficiency.And most wet processings all will use ammonia or ammonium salt.And the thorough recovery of ammonia nitrogen in waste water is relatively more difficult.So can cause ammonia and nitrogen pollution.
Summary of the invention
For solving the deficiencies in the prior art, the object of the present invention is to provide a kind of method for preparing cupric oxide, adopt raw material cheap and easy to get, improve production efficiency and product quality, and reduced the production cost of cupric oxide.
In order to realize described target, the present invention adopts following technical scheme: a kind of method for preparing cupric oxide is characterized in that: may further comprise the steps:
(1) injects in first container and contain Cu
2+Acidic solution, as stand-by liquid A;
(2) preparation contains CO in second container
3 2-And OH
-Solution, as stand-by liquid B;
(3) preparation contains CH in the 3rd container
3COO
-Solution, as stand-by liquid C;
(4) preparation contains OH in the 4th container
-Solution, as stand-by liquid D;
(5) stand-by liquid A, stand-by liquid B, stand-by liquid C are injected into carry out primary first-order equation in the 5th reactor, make the pH value of mixed solution E in the 5th reactor reach target pH value;
(6) desalination: after the reaction of (5) step finishes, in the 5th reactor, add stand-by liquid D, the pH value of solution value is after target pH value to the reactor, stop to add stand-by liquid D, and be warming up to target temperature, in the time period of reaction duration, keep the envrionment temperature of the 5th reactor at target temperature, reaction is down to room temperature after finishing;
(7) shift the desalination after product: step (6) products therefrom is transferred in the 6th reactor, and washs to washings and be neutral, carry out then tentatively making primary product except water treatment;
(8) preparation target product: in the 7th reactor, step (7) products therefrom is carried out processed, again it is transferred in the drying treatment device, under 50 ℃～150 ℃, carry out drying treatment, make the target product cupric oxide.
Aforementioned stand-by liquid A is Cu
2+Mass concentration is cupric chloride or the copper-bath of 0.5%-15%; Described stand-by liquid D is OH
-Mass concentration is the solubility oxyhydroxide of 1%-25%.
Solubility oxyhydroxide is at least a in potassium hydroxide, the sodium hydroxide among the aforementioned stand-by liquid D.
The mixing solutions that aforementioned stand-by liquid B is soluble carbon hydrochlorate and solubility oxyhydroxide, wherein CO
3 2-With OH
-Mol ratio is 1:0.5-2.
Soluble carbon hydrochlorate among the aforementioned stand-by liquid B is at least a in yellow soda ash, sodium bicarbonate, the salt of wormwood; Solubility oxyhydroxide is at least a in potassium hydroxide, the sodium hydroxide.
Cu among the aforementioned mixed solution E
2+With CH
3COO
-Mol ratio be 1:0.05-0.6.
In the abovementioned steps (5), one among stand-by liquid C and stand-by liquid A or the stand-by liquid B is mixed in intermediate receptacle in advance, mode with controllable flow speed is injected into not mixed stand-by liquid B or stand-by liquid A in the intermediate receptacle then, monitor the pH value of intermediate receptacle in real time, when arriving target pH value, stop to inject; Aforementioned target pH value scope is 6-8; Temperature of reaction control is at 45 ℃-90 ℃ in the abovementioned steps (5).
Target pH value scope is 10-14 in the abovementioned steps (6), and target temperature is 60 ℃-100 ℃, and the reaction duration is 30 minutes-2 hours, stops heating after reaction finishes, and opens water quench to room temperature after 30 minutes.
Aforementioned the 5th reactor is reactor, and the 6th reactor is vacuumfilter, and the 7th reactor is whizzer.
Usefulness of the present invention is: a kind of method for preparing cupric oxide provided by the invention, utilize cupric chloride, copper sulfate as raw material, and cupric chloride can obtain by handling discarded copper circuit board, or directly adopt the wiring board waste cuprous chloride solution, copper sulfate can be stripped by sulfuric acid by copper mine or waste cupron extraction and be got, so its cost of material is cheap relatively, adopts cheap and easy to get, nontoxic raw material, improve production efficiency and product quality, reduced the production cost of cupric oxide.
Embodiment
Below in conjunction with specific embodiment the present invention is done concrete introduction.
Reaction principle of the present invention is:
Embodiment 1:
(1) injects the acidic solution of sulfur acid copper in first container, as stand-by liquid A, the Cu in this solution
2+Mass concentration is 0.52%;
(2) in second container, prepare the mixing solutions that comprises yellow soda ash and sodium hydroxide, the CO in the solution
3 2-With OH
-Mol ratio is CO
3 2-: OH
-=1:0.5 is as stand-by liquid B;
(3) in the 3rd container, prepare acetum, as stand-by liquid C;
(4) in the 4th container, prepare sodium hydroxide solution, OH in the solution
-Mass concentration is 1%, as stand-by liquid D;
(5) add 500L water in the strap clamp of 2000L cover and the reactor that stirs, water temperature is 90 ℃; Stand-by liquid C is mixed in intermediate receptacle in advance with stand-by liquid A, make Cu
2+With CH
3COO
-Mol ratio Cu
2+: CH
3COO
-=1:0.05; With mixed solution and stand-by liquid B simultaneously, flow in the 5th reactor lentamente, adopt pH meter to monitor the pH value of solution in the 5th reactor in real time in the reaction process, the pH value in the reactor is controlled 6, obtain mixing solutions E;
(6) desalination: after (5) step reaction finishes, in the 5th reactor, add stand-by liquid D, to the reactor after the pH value of solution value to 10, stop to add stand-by liquid D, and be warming up to 100 ℃, insulation reaction 2 hours, stop heating after reaction finishes, open water quench to room temperature after 30 minutes;
(7) shift the desalination after product: step (6) the gained solid product that dewaters is put into the 6th reactor and carried out solid-liquid separation, the 6th reactor is vacuumfilter, be washed with water to washings again and be neutral, open vacuum then and carry out tentatively removing water treatment, make primary product;
(8) preparation target product: step (7) products therefrom is transferred in the 7th reactor, the 7th reactor is whizzer, it is carried out powerful dehydration handle, and it is transferred in the drying treatment device again, under 50 ℃, carry out drying treatment, make the target product cupric oxide.
Embodiment 2:
(1) in first container, injects the acidic solution that contains cupric chloride, as stand-by liquid A, the Cu in this solution
2+Mass concentration is 6.8%;
(2) in second container, prepare the mixing solutions that comprises sodium bicarbonate and sodium hydroxide, the CO in the solution
3 2-With OH
-Mol ratio is CO
3 2-: OH
-=1:1 is as stand-by liquid B;
(3) in the 3rd container, prepare liquor kalii acetici, as stand-by liquid C;
(4) in the 4th container, prepare potassium hydroxide solution, OH in the solution
-Mass concentration is 10%, as stand-by liquid D;
(5) add 500L water in the strap clamp of 2000L cover and the reactor that stirs, water temperature is 75 ℃; Stand-by liquid C is mixed in intermediate receptacle in advance with stand-by liquid B, make Cu
2+With CH
3COO
-Mol ratio Cu
2+: CH
3COO
-=1:0.2; With mixed solution and stand-by liquid A simultaneously, flow in the 5th reactor lentamente, adopt pH meter to monitor the pH value of solution in the 5th reactor in real time in the reaction process, the pH value in the reactor is controlled 7, obtain mixing solutions E;
(6) desalination: after (5) step reaction finishes, in the 5th reactor, add stand-by liquid D, to the reactor after the pH value of solution value to 11, stop to add stand-by liquid D, and be warming up to 90 ℃, insulation reaction 1.5 hours, stop heating after reaction finishes, open water quench to room temperature after 30 minutes;
(7) shift the desalination after product: step (6) the gained solid product that dewaters is put into the 6th reactor and carried out solid-liquid separation, the 6th reactor is vacuumfilter, be washed with water to washings again and be neutral, open vacuum then and carry out tentatively removing water treatment, make primary product;
(8) preparation target product: step (7) products therefrom is transferred in the 7th reactor, the 7th reactor is whizzer, it is carried out powerful dehydration handle, and it is transferred in the drying treatment device again, under 80 ℃, carry out drying treatment, make the target product cupric oxide.
Embodiment 3:
(1) injects the acidic solution of sulfur acid copper in first container, as stand-by liquid A, the Cu in this solution
2+Mass concentration is 9.8%;
(2) preparation comprises the mixing solutions of salt of wormwood and sodium hydroxide, potassium hydroxide, the CO in the solution in second container
3 2-With OH
-Mol ratio is CO
3 2-: OH
-=1:1.5 is as stand-by liquid B;
(3) in the 3rd container, prepare sodium acetate soln, as stand-by liquid C;
(4) preparation sodium hydroxide and potassium hydroxide mixing solutions in the 4th container, OH in the solution
-Mass concentration is 20%, as stand-by liquid D;
(5) add 500L water in the strap clamp of 2000L cover and the reactor that stirs, water temperature is 65 ℃; Stand-by liquid C is mixed in intermediate receptacle in advance with stand-by liquid B, make Cu
2+With CH
3COO
-Mol ratio Cu
2+: CH
3COO
-=1:0.4; With mixed solution and stand-by liquid A simultaneously, flow in the 5th reactor lentamente, adopt pH meter to monitor the pH value of solution in the 5th reactor in real time in the reaction process, the pH value in the reactor is controlled 7.5, obtain mixing solutions E;
(6) desalination: after (5) step reaction finishes, in the 5th reactor, add stand-by liquid D, to the reactor after the pH value of solution value to 12, stop to add stand-by liquid D, and be warming up to 80 ℃, insulation reaction 1 hour, stop heating after reaction finishes, open water quench to room temperature after 30 minutes;
(7) shift the desalination after product: step (6) the gained solid product that dewaters is put into the 6th reactor and carried out solid-liquid separation, the 6th reactor is vacuumfilter, be washed with water to washings again and be neutral, open vacuum then and carry out tentatively removing water treatment, make primary product;
(8) preparation target product: step (7) products therefrom is transferred in the 7th reactor, the 7th reactor is whizzer, it is carried out powerful dehydration handle, and it is transferred in the drying treatment device again, under 100 ℃, carry out drying treatment, make the target product cupric oxide.
Embodiment 4:
(1) in first container, injects the acidic solution that contains cupric chloride, as stand-by liquid A, the Cu in this solution
2+Mass concentration is 15%;
(2) in second container, prepare the mixing solutions that comprises sodium bicarbonate, yellow soda ash and potassium hydroxide, the CO in the solution
3 2-With OH
-Mol ratio is CO
3 2-: OH
-=1:2 is as stand-by liquid B;
(3) in the 3rd container, prepare liquor kalii acetici, as stand-by liquid C;
(4) in the 4th container, prepare sodium hydroxide solution, OH in the solution
-Mass concentration is 25%, as stand-by liquid D
(5) add 500L water in the strap clamp of 2000L cover and the reactor that stirs, water temperature is 45 ℃; Stand-by liquid C is mixed in intermediate receptacle in advance with stand-by liquid B, make Cu
2+With CH
3COO
-Mol ratio Cu
2+: CH
3COO
-=1:0.4; With mixed solution and stand-by liquid A simultaneously, flow in the 5th reactor lentamente, adopt pH meter to monitor the pH value of solution in the 5th reactor in real time in the reaction process, the pH value in the reactor is controlled 8, obtain mixing solutions E;
(6) desalination: after (5) step reaction finishes, in the 5th reactor, add stand-by liquid D, to the reactor after the pH value of solution value to 14, stop to add stand-by liquid D, and be warming up to 60 ℃, insulation reaction 30 minutes, stop heating after reaction finishes, open water quench to room temperature after 30 minutes;
(7) shift the desalination after product: step (6) the gained solid product that dewaters is put into the 6th reactor and carried out solid-liquid separation, the 6th reactor is vacuumfilter, be washed with water to washings again and be neutral, open vacuum then and carry out tentatively removing water treatment, make primary product;
(8) preparation target product: step (7) products therefrom is transferred in the 7th reactor, the 7th reactor is whizzer, it is carried out powerful dehydration handle, and it is transferred in the drying treatment device again, under 150 ℃, carry out drying treatment, make the target product cupric oxide.
Embodiment 1-4 is carried out sample master content analysis.Listed the result of test in the table 1.
Table 1 sample master content analysis
| Sample | Content (%) |
| Embodiment 1 | 98.3 |
| Embodiment 2 | 98.8 |
| Embodiment 3 | 99.2 |
| Embodiment 4 | 98.6 |
Quality product reaches GB/T674-78 standard, product content height as shown in Table 1.
More than show and described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand, and described embodiment does not limit the present invention in any form, and all employings are equal to replaces or technical scheme that the mode of equivalent transformation obtains, all drops in protection scope of the present invention.
Claims (9)
1. method for preparing cupric oxide is characterized in that: may further comprise the steps:
(1) injects in first container and contain Cu
2+Acidic solution, as stand-by liquid A;
(2) preparation contains CO in second container
3 2-And OH
-Solution, as stand-by liquid B;
(3) preparation contains CH in the 3rd container
3COO
-Solution, as stand-by liquid C;
(4) preparation contains OH in the 4th container
-Solution, as stand-by liquid D;
(5) stand-by liquid A, stand-by liquid B, stand-by liquid C are injected into carry out primary first-order equation in the 5th reactor, make the pH value of mixed solution E in the 5th reactor reach target pH value;
(6) desalination: after the reaction of (5) step finishes, in the 5th reactor, add stand-by liquid D, the pH value of solution value is after target pH value to the reactor, stop to add stand-by liquid D, and be warming up to target temperature, in the time period of reaction duration, keep the envrionment temperature of the 5th reactor at target temperature, reaction is down to room temperature after finishing;
(7) shift the desalination after product: step (6) products therefrom is transferred in the 6th reactor, and washs to washings and be neutral, carry out then tentatively making primary product except water treatment;
(8) preparation target product: in the 7th reactor, step (7) products therefrom is carried out processed, again it is transferred in the drying treatment device, under 50 ℃ ~ 150 ℃, carry out drying treatment, make the target product cupric oxide.
2. a kind of method for preparing cupric oxide according to claim 1, it is characterized in that: described stand-by liquid A is Cu
2+Mass concentration is cupric chloride or the copper-bath of 0.5%-15%; Described stand-by liquid D is OH
-Mass concentration is the solubility oxyhydroxide of 1%-25%.
3. according to a kind of method for preparing cupric oxide described in the claim 2, it is characterized in that: solubility oxyhydroxide is at least a in potassium hydroxide, the sodium hydroxide among the described stand-by liquid D.
4. according to a kind of method for preparing cupric oxide described in the claim 1, it is characterized in that: the mixing solutions that described stand-by liquid B is soluble carbon hydrochlorate and solubility oxyhydroxide, wherein CO
3 2-With OH
-Mol ratio is 1:0.5-2.
5. according to a kind of method for preparing cupric oxide described in the claim 4, it is characterized in that: the soluble carbon hydrochlorate among the described stand-by liquid B is at least a in yellow soda ash, sodium bicarbonate, the salt of wormwood; Solubility oxyhydroxide is at least a in potassium hydroxide, the sodium hydroxide.
6. a kind of method for preparing cupric oxide according to claim 1 is characterized in that: Cu among the described mixed solution E
2+With CH
3COO
-Mol ratio be 1:0.05-0.6.
7. according to each described a kind of method for preparing cupric oxide among the claim 1-6, it is characterized in that: in the described step (5), one among stand-by liquid C and stand-by liquid A or the stand-by liquid B is mixed in intermediate receptacle in advance, mode with controllable flow speed is injected into not mixed stand-by liquid B or stand-by liquid A in the intermediate receptacle then, monitor the pH value of intermediate receptacle in real time, when arriving target pH value, stop to inject; Described target pH value scope is 6-8; Temperature of reaction control is at 45 ℃-90 ℃ in the described step (5).
8. a kind of method for preparing cupric oxide according to claim 1, it is characterized in that: target pH value scope is 10-14 in the described step (6), target temperature is 60 ℃-100 ℃, the reaction duration is 30 minutes-2 hours, stop heating after reaction finishes, open water quench to room temperature after 30 minutes.
9. a kind of method for preparing cupric oxide according to claim 1, it is characterized in that: described the 5th reactor is reactor, and the 6th reactor is vacuumfilter, and the 7th reactor is whizzer.
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|---|---|---|---|
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|---|---|---|---|
| CN201310123321.6A CN103232056B (en) | 2013-04-10 | 2013-04-10 | Method of preparing copper oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496731A (en) * | 2013-09-11 | 2014-01-08 | 江西新金叶实业有限公司 | Method for preparing nanometer copper oxide by using copper scrap |
Citations (3)
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|---|---|---|---|---|
| CN101696027A (en) * | 2009-10-27 | 2010-04-21 | 中南民族大学 | Cubic copper oxide nano particle and synthesizing method and application thereof |
| CN102491402A (en) * | 2011-12-05 | 2012-06-13 | 广州科城环保科技有限公司 | Method for producing refined copper oxide by utilizing acidic waste etching solution |
| CN102491403A (en) * | 2011-12-19 | 2012-06-13 | 班朝磊 | Method for preparing copper oxide powder by using complexed-precipitation method |
-
2013
- 2013-04-10 CN CN201310123321.6A patent/CN103232056B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101696027A (en) * | 2009-10-27 | 2010-04-21 | 中南民族大学 | Cubic copper oxide nano particle and synthesizing method and application thereof |
| CN102491402A (en) * | 2011-12-05 | 2012-06-13 | 广州科城环保科技有限公司 | Method for producing refined copper oxide by utilizing acidic waste etching solution |
| CN102491403A (en) * | 2011-12-19 | 2012-06-13 | 班朝磊 | Method for preparing copper oxide powder by using complexed-precipitation method |
Non-Patent Citations (2)
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| 朱伟长 等: "氧化铜纳米粉的制备及分散方法", 《北京科技大学学报》 * |
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Cited By (1)
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|---|---|---|---|---|
| CN103496731A (en) * | 2013-09-11 | 2014-01-08 | 江西新金叶实业有限公司 | Method for preparing nanometer copper oxide by using copper scrap |
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