CN103232056B - Method of preparing copper oxide - Google Patents
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- CN103232056B CN103232056B CN201310123321.6A CN201310123321A CN103232056B CN 103232056 B CN103232056 B CN 103232056B CN 201310123321 A CN201310123321 A CN 201310123321A CN 103232056 B CN103232056 B CN 103232056B
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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, particularly relate to a kind of preparation method of cupric oxide.
Background technology
Cupric oxide of many uses, current main preparation methods is dry method and wet method.Active copper oxide is prepared primarily of wet processing, and the purposes of active copper oxide is also more extensive.But wet method preparation process a lot of at present, because the product granularity of cupric oxide is thin, causes the impurity after having prepared not utilize and washes, thus affect 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, production cost can be increased like this and have a strong impact on production efficiency.And most wet processing all will use ammonia or ammonium salt.And the thorough recovery of ammonia nitrogen in waste water is more difficult.So can ammonia and nitrogen pollution be caused.
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 preparing cupric oxide, adopting raw material cheap and easy to get, improve production efficiency and product quality, and reducing the production cost of cupric oxide.
In order to realize described target, the present invention adopts following technical scheme: a kind of method preparing cupric oxide, is characterized in that: comprise the following steps:
(1) inject containing Cu in the first container
2+acidic solution, as stand-by liquid A;
(2) in second container, preparation contains CO
3 2-and OH
-solution, as stand-by liquid B;
(3) in the 3rd container, preparation contains CH
3cOO
-solution, as stand-by liquid C;
(4) in the 4th container, preparation contains OH
-solution, as stand-by liquid D;
(5) stand-by liquid A, stand-by liquid B, stand-by liquid C are injected in the 5th reactor and carry out primary first-order equation, make the pH value of mixed solution E in the 5th reactor reach target ph;
(6) desalination: after (5) step reaction terminates, stand-by liquid D is added in the 5th reactor, to reactor after solution ph to target ph, stop adding stand-by liquid D, and be warming up to target temperature, within the time period of reaction duration, keep the envrionment temperature of the 5th reactor at target temperature, after reaction terminates, be down to room temperature;
(7) shift desalination after product: be transferred in the 6th reactor by step (6) products therefrom, and washing to washings is neutral, then carries out tentatively except water treatment, obtained primary product;
(8) prepare target product: in the 7th reactor, processed is carried out to step (7) products therefrom, then transfer them in drying processor, at 50 DEG C ~ 150 DEG C, carry out drying treatment, obtained 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 soluble hydroxide of 1%-25%.
In aforementioned stand-by liquid D, soluble hydroxide is at least one in potassium hydroxide, sodium hydroxide.
Aforementioned stand-by liquid B is the mixing solutions of soluble carbonate salt and soluble hydroxide, wherein CO
3 2-with OH
-mol ratio is 1:0.5-2.
Soluble carbonate salt in aforementioned stand-by liquid B is at least one in sodium carbonate, sodium bicarbonate, salt of wormwood; Soluble hydroxide is at least one in potassium hydroxide, sodium hydroxide.
Cu in aforementioned mixed solution E
2+with CH
3cOO
-mol ratio be 1:0.05-0.6.
In abovementioned steps (5), stand-by liquid C is mixed in intermediate receptacle in advance with in stand-by liquid A or stand-by liquid B, then in the mode of controllable flow speed, not mixed stand-by liquid B or stand-by liquid A is injected in intermediate receptacle, the pH value of Real-Time Monitoring intermediate receptacle, when arriving target ph, stop injecting; Preceding aim pH value range is 6-8; In abovementioned steps (5), temperature of reaction controls at 45 DEG C-90 DEG C.
In abovementioned steps (6), target ph scope is 10-14, and target temperature is 60 DEG C-100 DEG C, and reaction duration is 30 minutes-2 hours, and reaction terminates rear stopping heating, opens water quench to room temperature after 30 minutes.
Aforementioned 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 preparing cupric oxide provided by the invention, utilize cupric chloride, copper sulfate as raw material, and cupric chloride can be obtained by the copper circuit board that process is discarded, or directly adopt wiring board waste cuprous chloride solution, copper sulfate can obtain by stripping through sulfuric acid after copper mine or waste cupron extraction, so its cost of material relative moderate, adopts cheap and easy to get, nontoxic raw material, improve production efficiency and product quality, reduce the production cost of cupric oxide.
Embodiment
Below in conjunction with specific embodiment, concrete introduction is done to the present invention.
Reaction principle of the present invention is:
Embodiment 1:
(1) in the first container, the acidic solution of sulfur acid copper is injected, as stand-by liquid A, the Cu in this solution
2+mass concentration is 0.52%;
(2) in second container, preparation comprises the mixing solutions of sodium carbonate and sodium hydroxide, the CO in solution
3 2-with OH
-mol ratio is CO
3 2-: OH
-=1:0.5, as stand-by liquid B;
(3) in the 3rd container, acetum is prepared, as stand-by liquid C;
(4) in the 4th container, sodium hydroxide solution is prepared, OH in solution
-mass concentration is 1%, as stand-by liquid D;
(5) in the jacketed of 2000L and the reactor of stirring, add 500L water, water temperature is 90 DEG C; Stand-by liquid C is mixed in advance with stand-by liquid A in intermediate receptacle, makes Cu
2+with CH
3cOO
-mol ratio Cu
2+: CH
3cOO
-=1:0.05; Mixed solution and stand-by liquid B are flowed in the 5th reactor simultaneously, lentamente, adopts pH meter to monitor the pH value of solution in the 5th reactor in real time in reaction process, make the pH value in reactor control 6, obtain mixing solutions E;
(6) desalination: after (5) step reaction terminates, add stand-by liquid D, to reactor after solution ph to 10 in the 5th reactor, stop adding stand-by liquid D, and be warming up to 100 DEG C, insulation reaction 2 hours, reaction terminates rear stopping heating, opens water quench to room temperature after 30 minutes;
(7) desalination after product is shifted: the solid product that dewatered by step (6) gained is put into the 6th reactor and carried out solid-liquid separation, 6th reactor is vacuumfilter, be washed with water to washings again in neutral, then open vacuum and carry out tentatively except water treatment, obtained primary product;
(8) target product is prepared: be transferred to by step (7) products therefrom in the 7th reactor, 7th reactor is whizzer, carries out powerful dehydration process to it, then transfers them in drying processor, drying treatment is carried out, obtained target product cupric oxide at 50 DEG C.
Embodiment 2:
(1) in the first container, the acidic solution of containing copper chloride is injected, as stand-by liquid A, the Cu in this solution
2+mass concentration is 6.8%;
(2) in second container, preparation comprises the mixing solutions of sodium bicarbonate and sodium hydroxide, the CO in solution
3 2-with OH
-mol ratio is CO
3 2-: OH
-=1:1, as stand-by liquid B;
(3) in the 3rd container, liquor kalii acetici is prepared, as stand-by liquid C;
(4) in the 4th container, potassium hydroxide solution is prepared, OH in solution
-mass concentration is 10%, as stand-by liquid D;
(5) in the jacketed of 2000L and the reactor of stirring, add 500L water, water temperature is 75 DEG C; Stand-by liquid C is mixed in advance with stand-by liquid B in intermediate receptacle, makes Cu
2+with CH
3cOO
-mol ratio Cu
2+: CH
3cOO
-=1:0.2; Mixed solution and stand-by liquid A are flowed in the 5th reactor simultaneously, lentamente, adopts pH meter to monitor the pH value of solution in the 5th reactor in real time in reaction process, make the pH value in reactor control 7, obtain mixing solutions E;
(6) desalination: after (5) step reaction terminates, add stand-by liquid D, to reactor after solution ph to 11 in the 5th reactor, stop adding stand-by liquid D, and be warming up to 90 DEG C, insulation reaction 1.5 hours, reaction terminates rear stopping heating, opens water quench to room temperature after 30 minutes;
(7) desalination after product is shifted: the solid product that dewatered by step (6) gained is put into the 6th reactor and carried out solid-liquid separation, 6th reactor is vacuumfilter, be washed with water to washings again in neutral, then open vacuum and carry out tentatively except water treatment, obtained primary product;
(8) target product is prepared: be transferred to by step (7) products therefrom in the 7th reactor, 7th reactor is whizzer, carries out powerful dehydration process to it, then transfers them in drying processor, drying treatment is carried out, obtained target product cupric oxide at 80 DEG C.
Embodiment 3:
(1) in the first container, the acidic solution of sulfur acid copper is injected, as stand-by liquid A, the Cu in this solution
2+mass concentration is 9.8%;
(2) in second container, preparation comprises the mixing solutions of salt of wormwood and sodium hydroxide, potassium hydroxide, the CO in solution
3 2-with OH
-mol ratio is CO
3 2-: OH
-=1:1.5, as stand-by liquid B;
(3) in the 3rd container, sodium acetate soln is prepared, as stand-by liquid C;
(4) in the 4th container, sodium hydroxide and potassium hydroxide mixing solutions is prepared, OH in solution
-mass concentration is 20%, as stand-by liquid D;
(5) in the jacketed of 2000L and the reactor of stirring, add 500L water, water temperature is 65 DEG C; Stand-by liquid C is mixed in advance with stand-by liquid B in intermediate receptacle, makes Cu
2+with CH
3cOO
-mol ratio Cu
2+: CH
3cOO
-=1:0.4; Mixed solution and stand-by liquid A are flowed in the 5th reactor simultaneously, lentamente, adopts pH meter to monitor the pH value of solution in the 5th reactor in real time in reaction process, make the pH value in reactor control 7.5, obtain mixing solutions E;
(6) desalination: after (5) step reaction terminates, add stand-by liquid D, to reactor after solution ph to 12 in the 5th reactor, stop adding stand-by liquid D, and be warming up to 80 DEG C, insulation reaction 1 hour, reaction terminates rear stopping heating, opens water quench to room temperature after 30 minutes;
(7) desalination after product is shifted: the solid product that dewatered by step (6) gained is put into the 6th reactor and carried out solid-liquid separation, 6th reactor is vacuumfilter, be washed with water to washings again in neutral, then open vacuum and carry out tentatively except water treatment, obtained primary product;
(8) target product is prepared: be transferred to by step (7) products therefrom in the 7th reactor, 7th reactor is whizzer, carries out powerful dehydration process to it, then transfers them in drying processor, drying treatment is carried out, obtained target product cupric oxide at 100 DEG C.
Embodiment 4:
(1) in the first container, the acidic solution of containing copper chloride is injected, as stand-by liquid A, the Cu in this solution
2+mass concentration is 15%;
(2) in second container, preparation comprises the mixing solutions of sodium bicarbonate, sodium carbonate and potassium hydroxide, the CO in solution
3 2-with OH
-mol ratio is CO
3 2-: OH
-=1:2, as stand-by liquid B;
(3) in the 3rd container, liquor kalii acetici is prepared, as stand-by liquid C;
(4) in the 4th container, sodium hydroxide solution is prepared, OH in solution
-mass concentration is 25%, as stand-by liquid D
(5) in the jacketed of 2000L and the reactor of stirring, add 500L water, water temperature is 45 DEG C; Stand-by liquid C is mixed in advance with stand-by liquid B in intermediate receptacle, makes Cu
2+with CH
3cOO
-mol ratio Cu
2+: CH
3cOO
-=1:0.4; Mixed solution and stand-by liquid A are flowed in the 5th reactor simultaneously, lentamente, adopts pH meter to monitor the pH value of solution in the 5th reactor in real time in reaction process, make the pH value in reactor control 8, obtain mixing solutions E;
(6) desalination: after (5) step reaction terminates, add stand-by liquid D, to reactor after solution ph to 14 in the 5th reactor, stop adding stand-by liquid D, and be warming up to 60 DEG C, insulation reaction 30 minutes, reaction terminates rear stopping heating, opens water quench to room temperature after 30 minutes;
(7) desalination after product is shifted: the solid product that dewatered by step (6) gained is put into the 6th reactor and carried out solid-liquid separation, 6th reactor is vacuumfilter, be washed with water to washings again in neutral, then open vacuum and carry out tentatively except water treatment, obtained primary product;
(8) target product is prepared: be transferred to by step (7) products therefrom in the 7th reactor, 7th reactor is whizzer, carries out powerful dehydration process to it, then transfers them in drying processor, drying treatment is carried out, obtained target product cupric oxide at 150 DEG C.
The main content analysis of sample is carried out to embodiment 1-4.The result of test is listed in table 1.
The main content analysis of table 1 sample
| 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 as shown in Table 1, and product content is high.
More than show and describe 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, the technical scheme that the mode that all employings are equal to replacement or equivalent transformation obtains, and all drops in protection scope of the present invention.
Claims (2)
1. prepare a method for cupric oxide, it is characterized in that: comprise the following steps:
(1) inject containing Cu in the first container
2+acidic solution, as stand-by liquid A;
(2) in second container, preparation contains CO
3 2-and OH
-solution, as stand-by liquid B;
(3) in the 3rd container, preparation contains CH
3cOO
-solution, as stand-by liquid C;
(4) in the 4th container, preparation contains OH
-solution, as stand-by liquid D;
(5) stand-by liquid A, stand-by liquid B, stand-by liquid C are injected in the 5th reactor and carry out primary first-order equation, make the pH value of mixed solution E in the 5th reactor reach target ph;
(6) desalination: after (5) step reaction terminates, stand-by liquid D is added in the 5th reactor, to reactor after solution ph to target ph, stop adding stand-by liquid D, and be warming up to target temperature, within the time period of reaction duration, keep the envrionment temperature of the 5th reactor at target temperature, after reaction terminates, be down to room temperature;
(7) shift desalination after product: be transferred in the 6th reactor by step (6) products therefrom, and washing to washings is neutral, then carries out tentatively except water treatment, obtained primary product;
(8) prepare target product: in the 7th reactor, processed is carried out to step (7) products therefrom, then transfer them in drying processor, at 50 DEG C ~ 150 DEG C, carry out drying treatment, obtained target product cupric oxide; Cu in described mixed solution E
2+with CH
3cOO
-mol ratio be 1:0.05-0.6; 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 soluble hydroxide of 1%-25%; In described stand-by liquid D, soluble hydroxide is at least one in potassium hydroxide, sodium hydroxide; Described stand-by liquid B is the mixing solutions of soluble carbonate salt and soluble hydroxide, wherein CO
3 2-with OH
-mol ratio is 1:0.5-2; Soluble carbonate salt in described stand-by liquid B is at least one in sodium carbonate, sodium bicarbonate, salt of wormwood; Soluble hydroxide is at least one in potassium hydroxide, sodium hydroxide; In described step (5), stand-by liquid C is mixed in intermediate receptacle in advance with in stand-by liquid A or stand-by liquid B, then in the mode of controllable flow speed, not mixed stand-by liquid B or stand-by liquid A is injected in intermediate receptacle, the pH value of Real-Time Monitoring intermediate receptacle, when arriving target ph, stop injecting; Described target ph scope is 6-8; In described step (5), temperature of reaction controls at 45 DEG C-90 DEG C; In described step (6), target ph scope is 10-14, and target temperature is 60 DEG C-100 DEG C, and reaction duration is 30 minutes-2 hours, and reaction terminates rear stopping heating, opens water quench to room temperature after 30 minutes.
2. a kind of method preparing cupric oxide according to claim 1, is characterized in that: described 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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| CN103232056B true CN103232056B (en) | 2015-04-15 |
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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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| 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)
| Title |
|---|
| 氧化铜纳米微粒的制备方法;胡静 等;《化工中间体》;20101231(第9期);第12-15页 * |
| 氧化铜纳米粉的制备及分散方法;朱伟长 等;《北京科技大学学报》;20030630;第25卷(第3期);第251-253页 * |
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