CN103232055B - Method of preparing basic copper carbonate - Google Patents

Method of preparing basic copper carbonate Download PDF

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CN103232055B
CN103232055B CN201310123585.1A CN201310123585A CN103232055B CN 103232055 B CN103232055 B CN 103232055B CN 201310123585 A CN201310123585 A CN 201310123585A CN 103232055 B CN103232055 B CN 103232055B
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CN103232055A (en
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廖勇志
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Suzhou Long Lake Nano Science And Technology Co ltd
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Abstract

The present invention provides a method of preparing basic copper carbonate, comprising the steps of: injecting a Cu<2+> containing acidic solution, a CO3<2-> and OH<-> containing solution and a CH3COO<-> containing solution into a container for a primary reaction, and performing washing and preliminary dehydration treatments to a solid product in the mixed solution to obtain a water containing solid product; and after performing a powerful dehydration treatment, drying at a temperature of 50 DEG C -150 DEG C to obtain the target product basic copper carbonate. 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 basic copper carbonate.

Description

A kind of method preparing ventilation breather
Technical field
The present invention relates to chemical production field, particularly relate to the preparation method of ventilation breather.
Background technology
Ventilation breather has another name called copper carbonate, of many uses.Such as organic catalyst compound, electroplating industry electroplating copper tin alloy make the additive, public nuisance-free agricultural chemicals, fodder additives etc. of cupric ion.Existing is that ventilation breather prepared by raw material with copper sulfate because cost height difficulty meet the need of market.Therefore the ventilation breather manufacture method finding a kind of more low cost more meets the development trend in market.
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 ventilation breather, adopting raw material cheap and easy to get, improve production efficiency and product quality, reducing the production cost of ventilation breather.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
Prepare a method for ventilation breather, 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) stand-by liquid A, stand-by liquid B, stand-by liquid C are injected in the 4th container and carry out primary first-order equation, make the pH value of mixed solution D in the 4th container reach target ph;
(5) solid product in mixed solution D is transferred in the 5th container, washing is carried out to washings used in neutral to it, then carrying out vacuum filtration tentatively except water treatment to passing through the solid product washed, obtaining aqueous solid product;
(6) target product is prepared: step (5) gained aqueous solid product is put into the 6th reactor, carries out powerful dehydration process, then transfer them in drying processor, at 50 DEG C-150 DEG C, carry out drying treatment, obtained target product basic copper carbonate.
Aforementioned stand-by liquid A is Cu 2+mass concentration is cupric chloride, the copper-bath of 0.5%-15%.
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.
Aforementioned stand-by liquid C is at least one in acetic acid, solubility acetate, and above-mentioned solubility acetate is at least one in sodium-acetate, Potassium ethanoate.
Cu in aforementioned mixed solution D 2+with CH 3cOO -mol ratio be 1:0.05-0.6.
In abovementioned steps (4), 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; Above-mentioned target ph scope is 6-8; In abovementioned steps (4), temperature of reaction controls at 45 DEG C-90 DEG C.
Aforementioned 4th container is reactor, and the 5th container is suction filter, and the 6th reactor is whizzer.
Usefulness of the present invention is: 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, adopt cheap and easy to get, nontoxic raw material, improve production efficiency and product quality, reduce the production cost of ventilation breather.
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 containing copper chloride 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 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 4th reactor simultaneously, lentamente, adopts pH meter to monitor the pH value of solution in the 4th reactor in real time in reaction process, make the pH value in reactor control 6, obtain mixing solutions D;
(5) be transferred to by the solid product in mixed solution D in the 5th container, the 5th container is suction filter, carries out washing to washings used in neutral to it, then carrying out vacuum filtration tentatively except water treatment to passing through the solid product washed, obtaining aqueous solid product;
(6) step (5) gained aqueous solid product is put into the 6th reactor, the 6th reactor is whizzer, carries out powerful dehydration process, then transfers them in drying processor, at 50 DEG C, carry out drying treatment, obtained target product basic copper carbonate.
Embodiment 2:
(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 6.3%;
(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 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 4th reactor simultaneously, lentamente, adopts pH meter to monitor the pH value of solution in the 4th reactor in real time in reaction process, make the pH value in reactor control 7, obtain mixing solutions D;
(5) be transferred to by the solid product in mixed solution D in the 5th container, the 5th container is suction filter, carries out washing to washings used in neutral to it, then carrying out vacuum filtration tentatively except water treatment to passing through the solid product washed, obtaining aqueous solid product;
(6) step (5) gained aqueous solid product is put into the 6th reactor, the 6th reactor is whizzer, carries out powerful dehydration process, then transfers them in drying processor, at 80 DEG C, carry out drying treatment, obtained target product basic copper carbonate.
Embodiment 3:
(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 10.5%;
(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 jacketed of 2000L and the reactor of stirring, add 500L water, water temperature is 55 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 4th reactor simultaneously, lentamente, adopts pH meter to monitor the pH value of solution in the 4th reactor in real time in reaction process, make the pH value in reactor control 7.5, obtain mixing solutions D;
(5) be transferred to by the solid product in mixed solution D in the 5th container, the 5th container is suction filter, carries out washing to washings used in neutral to it, then carrying out vacuum filtration tentatively except water treatment to passing through the solid product washed, obtaining aqueous solid product;
(6) step (5) gained aqueous solid product is put into the 6th reactor, the 6th reactor is whizzer, carries out powerful dehydration process, then transfers them in drying processor, at 100 DEG C, carry out drying treatment, obtained target product basic copper carbonate.
Embodiment 4:
(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 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 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 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 4th reactor simultaneously, lentamente, adopts pH meter to monitor the pH value of solution in the 4th reactor in real time in reaction process, make the pH value in reactor control 8, obtain mixing solutions D;
(5) be transferred to by the solid product in mixed solution D in the 5th container, the 5th container is suction filter, carries out washing to washings used in neutral to it, then carrying out vacuum filtration tentatively except water treatment to passing through the solid product washed, obtaining aqueous solid product;
(6) step (5) gained aqueous solid product is put into the 6th reactor, 6th reactor is powerful dehydration device, carries out powerful dehydration process, then transfers them in drying processor, drying treatment is carried out, obtained target product basic copper carbonate at 150 DEG C.
Main content analysis is carried out to the sample that embodiment 1-4 prepares.The result of test is listed in table 1.
The main content of table 1 sample
Sample Copper content (%)
Embodiment 1 55.2
Embodiment 2 55.8
Embodiment 3 56.3
Embodiment 4 55.6
The quality product of embodiment 1-4 reaches G/321283GY03-2002 standard as shown in Table 1, and quality product 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 above-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 ventilation breather, 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) stand-by liquid A, stand-by liquid B, stand-by liquid C are injected in the 4th container and carry out primary first-order equation, make the pH value of mixed solution D in the 4th container reach target ph;
(5) solid product in mixed solution D is transferred in the 5th container, washing is carried out to washings used in neutral to it, then carrying out vacuum filtration tentatively except water treatment to passing through the solid product washed, obtaining aqueous solid product;
(6) target product is prepared: step (5) gained aqueous solid product is put into the 6th reactor, carries out powerful dehydration process, then transfer them in drying processor, at 50 DEG C-150 DEG C, carry out drying treatment, obtained target product basic copper carbonate; Cu in above-mentioned mixed solution D 2+with CH 3cOO -mol ratio be 1:0.05-0.6; Above-mentioned stand-by liquid A is Cu 2+mass concentration is cupric chloride, the copper-bath of 0.5%-15%; Above-mentioned 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 above-mentioned 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; Above-mentioned stand-by liquid C is at least one in acetic acid, solubility acetate, and above-mentioned solubility acetate is at least one in sodium-acetate, Potassium ethanoate; In above-mentioned steps (4), 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; Above-mentioned target ph scope is 6-8; In above-mentioned steps (4), temperature of reaction controls at 45 DEG C-90 DEG C.
2. a kind of method preparing ventilation breather according to claim 1, is characterized in that, above-mentioned 4th container is reactor, and the 5th container is suction filter, and the 6th reactor is whizzer.
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CN105060331B (en) * 2015-08-15 2017-03-01 淮北师范大学 A kind of preparation method of the micro-nano hierarchy of controllable basic copper carbonate
CN105293559A (en) * 2015-11-23 2016-02-03 上海应用技术学院 High-purity basic cupric carbonate microsphere and preparation method
CN105314668B (en) * 2015-11-23 2018-01-16 东莞市广华化工有限公司 A kind of method from circuit board acidic etching waste liquor recovery basic copper carbonate
CN106976902A (en) * 2016-11-30 2017-07-25 佛山市兴华源机械设备有限公司 A kind of method for preparing basic copper carbonate using industrial copper-containing etching waste solution
CN107311219B (en) * 2017-07-18 2019-07-02 清华大学 The method of purification of chessy copper pigment
CN107324373B (en) * 2017-07-18 2019-05-28 清华大学 The method of purification of malachite pigment
CN109987653A (en) * 2017-12-29 2019-07-09 荆门市格林美新材料有限公司 A kind of preparation method of near-spherical basic nickel carbonate
CN111747439B (en) * 2020-07-13 2023-08-29 泰兴冶炼厂有限公司 Preparation process of ultra-high sodium carbonate copper carbonate

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Effective date of registration: 20160511

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