Method for preparing electroplating-grade copper sulfate pentahydrate by aerosol technology

Abstract

The invention relates to the technical field of chemistry and inorganic chemical industry, in particular to a method for preparing electroplating-grade copper sulfate pentahydrate through an aerosol technology. The method comprises the following steps: mixing and stirring industrial-grade basic cupric carbonate and water, and discharging an upper-layer solution to obtain washed basic cupric carbonate; adding the washed basic cupric carbonate into a copper ion saturated solution, centrifuging, and discharging an upper solution to obtain refined basic cupric carbonate; uniformly mixing the refined basic cupric carbonate with a glucose aqueous solution, then adding an alkali solution for reaction, and discharging supernatant liquid to obtain a first mixture; mixing the first mixture with copper sulfate mother liquor, adding concentrated acid, and reacting to obtain first mother liquor; and preparing the first mother liquor into aerosol, taking the aerosol out by carrier gas, and heating the aerosol on a substrate to generate electroplating-grade copper sulfate pentahydrate in situ. The method disclosed by the invention is simple and has the characteristics of small opening flow of mother liquor, low water demand, few impurity removal processes, simple steps and high direct recovery rate of copper.

Description

Technical Field

[0001] The invention relates to the technical field of chemistry and inorganic chemical industry, and in particular to a method for preparing electroplating-grade copper sulfate pentahydrate by using aerosol technology. Background Art

[0002] At present, the preparation of electroplating grade copper sulfate pentahydrate mainly includes the copper hydroxide intermediate method and the copper oxide intermediate method. The former is to prepare the copper hydroxide intermediate by reacting basic copper chloride with ammonia water, and then add sulfuric acid to acidify and prepare copper sulfate after washing away the copper ammonia solution. This method uses relatively cheap ammonia water as the reaction raw material, and the copper ammonia solution byproduct can be used to synthesize basic copper chloride, but a large amount of ammonia gas is generated during the preparation of the intermediate, and the waste gas treatment is more troublesome, the production equipment investment is high, and the direct copper recovery rate is only 72% to 74%, and a large amount of copper is left in the copper ammonia solution. The latter is to prepare the copper oxide intermediate using copper-containing waste liquid, and then react with concentrated sulfuric acid to prepare copper sulfate after washing away soluble impurities. This method has a high direct copper recovery rate and good copper sulfate product quality, but it has the disadvantages of large wastewater generation, large amount of water required for multiple washings of the intermediate, and long production time.

[0003] Chinese patent CN202110209337.3 discloses a preparation method for preparing electroplating grade copper sulfate pentahydrate using crude basic copper carbonate, using crude basic copper carbonate to wash with pure water: basic copper carbonate mass ratio of 1:2, centrifugation and adding copper ion saturated acid solution of pH=2 according to copper ion saturated solution: basic copper carbonate mass ratio=1:2, secondary centrifugation to obtain refined basic copper carbonate, add 35L pure water and 5kg refined basic copper carbonate in the reactor, slowly add 2.5L concentrated sulfuric acid at 200ml / min, transfer to the crystallization tank after adding, and obtain electroplating grade copper sulfate pentahydrate wet product after multiple crystallization centrifugation operations, and then obtain electroplating grade copper sulfate pentahydrate after drying at 40°C. The copper sulfate pentahydrate prepared by this method has high purity and less insoluble matter, but there are more impurity removal processes, resulting in more water required for the experiment and a larger mother liquor opening flow.

[0004] Chinese patent CN202311249760.1 discloses a method for preparing electroplating grade copper sulfate pentahydrate, and the specific steps are as follows: industrial-grade basic copper chloride screens out fine material, adds water to pulp, adds NaOH solution, stirs and reacts for 1 to 3 hours under the conditions of pH 11 to 13 and temperature 60 to 80 ° C, filters out crude copper oxide, and washes with water 4 times to obtain a copper oxide intermediate. The copper oxide intermediate is slurried by adding water or copper sulfate mother liquor, and then added with concentrated sulfuric acid to acidify, and the pH of the reaction end point is controlled to be 1.6 to 2.2, oxidized and impurities are removed, filtered while hot, and the filtrate is cooled and crystallized, and the crude copper sulfate is filtered out, and then washed, dried, sieved and other steps are performed in sequence to obtain an electroplating grade copper sulfate pentahydrate product. The copper sulfate pentahydrate prepared by this method has a high purity and less insoluble matter, but the steps are cumbersome, the production is time-consuming, and the experimental water is more. Summary of the invention

[0005] Aiming at the shortcomings of the prior art of preparing electroplating-grade copper sulfate, such as large amount of waste water generated from multiple washings, easy exceeding of impurity content in the product, large mother liquor flow rate and low direct copper recovery rate, the present invention provides a method for preparing electroplating-grade copper sulfate pentahydrate using aerosol technology.

[0006] To achieve the above object, the present invention provides the following solutions:

[0007] One of the technical solutions of the present invention is a method for preparing electroplating grade copper sulfate pentahydrate using aerosol technology, comprising the following steps:

[0008] Mixing industrial-grade basic copper carbonate with water and stirring, and then discharging the upper solution to obtain water-washed basic copper carbonate;

[0009] adding the washed basic copper carbonate to a copper ion saturated solution, centrifuging and discharging the upper layer solution to obtain refined basic copper carbonate;

[0010] The refined basic copper carbonate and the glucose aqueous solution are mixed evenly, then an alkali solution is added to react, and the supernatant is discharged to obtain a first mixture;

[0011] The first mixture is mixed with copper sulfate mother liquor, and concentrated acid is added to react to obtain a first mother liquor;

[0012] The first mother liquid is prepared into an aerosol; the aerosol is carried out by a carrier gas and then heated to generate the electroplating grade copper sulfate pentahydrate in situ on a substrate.

[0013] A second technical solution of the present invention is an electroplating-grade copper sulfate pentahydrate prepared according to the above method.

[0014] A third technical solution of the present invention is the use of the above-mentioned electroplating-grade copper sulfate pentahydrate in electroplating.

[0015] The present invention discloses the following technical effects:

[0016] The present invention provides a method for preparing electroplating grade copper sulfate pentahydrate by aerosol technology. The method is simple and has the characteristics of small mother liquor flow rate, small water requirement, few impurity removal processes, simple steps and high copper direct recovery rate. The electroplating grade copper sulfate pentahydrate prepared by the method has high purity and uniform particle size distribution. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0018] Figure 1 The figure is a schematic diagram of the process flow for preparing electroplating grade copper sulfate pentahydrate by the aerosol technology of the present invention.

[0019] Figure 2 This is a SEM image of electroplating grade copper sulfate pentahydrate prepared by the method of specific example 2.

[0020] Figure 3 This is a particle size distribution diagram of electroplating grade copper sulfate pentahydrate prepared by the method of specific embodiment 3. DETAILED DESCRIPTION

[0021] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as limiting the present invention, but should be understood as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0022] It should be understood that the terms described in the present invention are only for describing a particular embodiment and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. The intermediate value in any stated value or stated range, and each smaller range between any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0023] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials associated with the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail.

[0024] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments of the present invention description without departing from the scope or spirit of the present invention. Other embodiments derived from the present invention description will be apparent to the skilled artisan. The present invention description and examples are exemplary only.

[0025] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0026] The "%" described in the present invention, unless otherwise specified, refers to mass percentage.

[0027] The first aspect of the present invention provides a method for preparing electroplating grade copper sulfate pentahydrate using aerosol technology, comprising the following steps:

[0028] Step 1, mixing industrial-grade basic copper carbonate with water, stirring, and then discharging the upper layer solution to obtain water-washed basic copper carbonate;

[0029] adding the washed basic copper carbonate to a copper ion saturated solution, centrifuging and discharging the upper layer solution to obtain refined basic copper carbonate;

[0030] Step 2, mixing the refined basic copper carbonate and the glucose aqueous solution uniformly, then adding an alkaline solution to react, and discharging the supernatant to obtain a first mixture;

[0031] Step 3, mixing the first mixture with copper sulfate mother liquor, and then adding concentrated acid to react to obtain a first mother liquor;

[0032] Step 4, preparing the first mother solution into an aerosol; the aerosol is carried out by the carrier gas and then heated on the substrate to generate the electroplating grade copper sulfate pentahydrate in situ.

[0033] In a preferred embodiment of the present invention, the pH of the saturated copper ion solution is 0-5, and more preferably 2; the saturated copper ion solution is a saturated solution of copper salt (such as copper chloride, copper nitrate, copper formate saturated solution, etc.), and more preferably copper chloride and copper nitrate.

[0034] In a preferred embodiment of the present invention, the mass ratio of the water-washed basic copper carbonate to the copper ion saturated solution is (0.5-2):1, and more preferably 1.5:1.

[0035] In a preferred embodiment of the present invention, the refined basic copper carbonate further includes the step of dispersing the refined basic copper carbonate into water before mixing with the glucose aqueous solution; the mass volume ratio of the refined basic copper carbonate to water is 1g:4ml; the concentration of the glucose aqueous solution is 2mol / L; the molar mass ratio of glucose in the glucose aqueous solution to the refined basic copper carbonate is 1mol:(20-120)g, and more preferably 1mol:120g; the alkaline solution is a sodium hydroxide aqueous solution with a concentration of 7.5mol / L; the volume ratio of the glucose aqueous solution to the alkaline solution is (3-5):1, and more preferably 50:13.

[0036] The ratio of glucose to refined basic copper carbonate should not be too small, because glucose as a reducing agent can reduce the divalent copper in refined basic copper carbonate to monovalent copper in cuprous oxide. If the ratio is too small, the reduction effect is poor, and the generated cuprous oxide is impure, which leads to a low yield when preparing copper sulfate pentahydrate. When the amount of glucose is too much, the effect of improving the yield of copper sulfate pentahydrate is not obvious, so considering the comprehensive effect and cost, the present invention preferably limits the amount of glucose aqueous solution to the above ratio range.

[0037] In the present invention, refined basic copper carbonate is mixed with a glucose aqueous solution, and then an alkali solution is added to react to obtain brick-red cuprous oxide.

[0038] In the step 1 and the step 2, a centrifugal separation step is also included before discharging the upper solution or the upper clear liquid.

[0039] In a preferred embodiment of the present invention, the copper ion content in the copper sulfate mother liquor is 70 g / L and the pH is 1.50.

[0040] In a preferred embodiment of the present invention, the mass ratio of the copper sulfate mother liquor to the first mixture is 15 ml:1 g; the concentrated acid is concentrated sulfuric acid; and the mass volume ratio of the first mixture to the concentrated acid is 10 g:(13-17) ml.

[0041] In a preferred embodiment of the present invention, the first mother liquid is prepared into an aerosol by an ultrasonic atomization powder making device.

[0042] In a preferred embodiment of the present invention, the carrier gas includes carrier gas a and carrier gas b; the carrier gas a is air; the carrier gas b is air; the flow rate of the carrier gas a is 450 sccm; the flow rate of the carrier gas b is 50 sccm; the heating temperature is 70°C; and the substrate is a glass substrate.

[0043] If the flow rate of carrier gas a is too small, the preparation speed will be too slow, and the particle size of the finished electroplating-grade copper sulfate pentahydrate will be larger. If it is too large, the reaction speed will be too fast, affecting the reaction time and reducing the content of electroplating-grade copper sulfate pentahydrate.

[0044] The flow rate of carrier gas b will affect the reaction speed. If the flow rate is too large, the reaction speed will be fast, but the reaction is likely to be incomplete. If the flow rate is too small, the reaction speed will be slow, affecting the microscopic morphology of the electroplating grade copper sulfate pentahydrate product and making it easy to agglomerate.

[0045] A second aspect of the present invention provides an electroplating grade copper sulfate pentahydrate prepared according to the above method.

[0046] The third aspect of the present invention provides the use of the electroplating grade copper sulfate pentahydrate in electroplating.

[0047] The process flow diagram of the present invention for preparing electroplating grade copper sulfate pentahydrate by aerosol technology is as follows Figure 1 shown.

[0048] Unless otherwise specified, the raw materials used in the embodiments of the present invention can be obtained through commercial sources.

[0049] The present invention is further described below by way of examples.

[0050] The following examples of the present invention are laboratory preparation cases, which are prepared using conventional laboratory instruments.

[0051] Example 1

[0052] Step 1, take 200g of industrial-grade basic copper carbonate with an iron content of 100ppm and a copper content of 58%, add 200g of pure water, stir continuously at a speed of 200rpm / min for 30min, centrifuge, discharge the upper solution, obtain washed basic copper carbonate, dissolve excess cupric chloride in water to form a copper ion saturated solution, add hydrochloric acid dropwise to adjust the saturated solution pH to 2.5, add 200g of washed basic copper carbonate to 100g of the copper ion saturated solution, centrifuge at 1000r / min for 30min, separate, discharge the upper solution, and obtain refined basic copper carbonate. The copper content in the refined basic copper carbonate is 64%.

[0053] Step 2, add 1L of 2mol / L glucose aqueous solution to the first reactor, disperse 120g of refined basic copper carbonate into 500ml of pure water and add it to the first reactor and stir evenly at 160r / min, add 250ml of 7.5mol / L sodium hydroxide aqueous solution to the first reactor while stirring, adjust the temperature in the first reactor to 60°C after mixing evenly, react for 30min, and after the reaction is completed, centrifuge and discharge the supernatant to obtain a first mixture.

[0054] Step 3, add 1.5L copper sulfate mother liquor into the second reactor, the copper ion content of the copper sulfate mother liquor is 70g / L, the pH is 1.50, the calcium content is 263ppm, and the chlorine content is 821ppm, and 100g of the first mixture is added into the second reactor while stirring, and the temperature of the second reactor is adjusted to 30°C, and 150ml of concentrated sulfuric acid is slowly added to react for 30min, at which time the mixed reaction system will release a large number of bubbles, and after the reaction is completed, the first mother liquor is obtained. It is dark blue and transparent, the temperature is 68°C, and the copper ion concentration is 164g / L.

[0055] Step 4, the first mother liquor is transferred to an ultrasonic atomization powder making device, the device parameters are adjusted, the ultrasonic frequency is 1.9MHz, an aerosol is formed, the flow rate of carrier gas a (air) is adjusted to 250sccm, the flow rate of carrier gas b (air) is set to 30sccm, the aerosol is taken out by carrier gas a, protected by carrier gas b, and then passed through a 60°C heating device to generate copper sulfate pentahydrate in situ on a 30°C slightly heated PET substrate, and the product is collected to obtain electroplating grade copper sulfate pentahydrate. The direct yield of the obtained product reaches 84.7%.

[0056] The electroplating grade copper sulfate pentahydrate prepared in this embodiment was tested for metal impurities and chloride ion content. The metal impurities were detected by ICP-OES method with a detection limit of 0.0003%; the chloride ion content was detected by UV-Vis method with a detection limit of 0.001%. The specific test results are shown in Table 1 below:

[0057] Table 1

[0058]

[0059] Note: ND means not detected; the same as in the following table.

[0060] Electroplating grade copper sulfate pentahydrate requires that the metal impurity content is less than 5ppm and the chlorine impurity content is less than 20ppm. As shown in Table 1, the electroplating grade copper sulfate pentahydrate prepared in this embodiment meets the requirements.

[0061] Example 2

[0062] Step 1, take 1kg of industrial-grade basic copper carbonate with an iron content of 400ppm and a copper content of 54%, add 1kg of pure water, stir continuously at a speed of 400rpm / min for 30min, centrifuge, discharge the upper solution, obtain washed basic copper carbonate, dissolve excess copper nitrate in water to form a copper ion saturated solution, add nitric acid dropwise to adjust the saturated solution pH to 0.1, add 750g of washed basic copper carbonate to 500g of the copper ion saturated solution, centrifuge at 2000r / min for 30min, separate, discharge the upper solution, and obtain refined basic copper carbonate. The copper content in the refined basic copper carbonate is 61%.

[0063] Step 2, add 5L of 2mol / L glucose aqueous solution to the first reactor, disperse 1.2kg of refined basic copper carbonate into 2.5L of pure water and add it to the first reactor and stir evenly at 200r / min, while stirring, add 1.3L of 7.5mol / L sodium hydroxide aqueous solution to the first reactor, adjust the temperature in the first reactor to 60°C after mixing evenly, react for 30min, and after the reaction is completed, centrifuge and discharge the supernatant to obtain a first mixture.

[0064] Step 3, add 7.5L copper sulfate mother liquor into the second reactor, the copper ion content of the copper sulfate mother liquor is 70g / L, the pH is 1.50, the calcium content is 263ppm, and the chlorine content is 821ppm, and 500g of the first mixture is added into the second reactor while stirring, and the temperature of the second reactor is adjusted to 30°C, and 750ml of concentrated sulfuric acid is slowly added to react for 30min, at which time the mixed reaction system will release a large number of bubbles, and after the reaction is completed and the concentrated sulfuric acid is added, the first mother liquor is obtained. It is dark blue and transparent, the temperature is 66°C, and the copper ion concentration is 173g / L.

[0065] Step 4, the first mother liquor is transferred to an ultrasonic atomization powder making device, the device parameters are adjusted, the ultrasonic frequency is 2.4MHz, an aerosol is formed, the flow rate of carrier gas a (air) is adjusted to 450sccm, the flow rate of carrier gas b (air) is set to 50sccm, the aerosol is taken out by carrier gas a, protected by carrier gas b, and then passed through a 70°C heating device to generate copper sulfate pentahydrate in situ on a 40°C micro-heated glass substrate, and the product is collected to obtain electroplating grade copper sulfate pentahydrate. The direct yield of the obtained product reaches 86.6%.

[0066] The above operation was repeated three times, and the prepared products were all mixed and sampled for inspection. The results are shown in Table 2:

[0067] Table 2

[0068]

[0069]

[0070] As shown in Table 2, the copper sulfate product prepared by the method of the present invention has stable quality, and all indicators meet the high-quality standards of electroplating-grade copper sulfate pentahydrate.

[0071] Figure 2 This is a SEM image of the electroplating grade copper sulfate pentahydrate prepared in Example 2. Figure 2 It can be seen that the electroplating-grade copper sulfate pentahydrate prepared in this embodiment has a uniform particle size distribution.

[0072] Example 3

[0073] Step 1, take 2kg of industrial-grade basic copper carbonate with an iron content of 300ppm and a copper content of 56%, add 2kg of pure water, stir continuously at a speed of 300rpm / min for 30min, centrifuge, discharge the upper solution to obtain washed basic copper carbonate, dissolve excess copper formate in water to form a copper ion saturated solution, add formic acid to adjust the saturated solution pH to 4.1, add 750g of washed basic copper carbonate to 1kg of copper ion saturated solution, centrifuge at 1500r / min for 30min, separate, discharge the upper solution, and obtain refined basic copper carbonate. The copper content in the refined basic copper carbonate is 63%.

[0074] Step 2, add 10L of 2mol / L glucose aqueous solution to the first reactor, disperse 1.2kg of refined basic copper carbonate into 5L of pure water and add it to the first reactor and stir evenly at 300r / min, add 2.5L of 7.5mol / L sodium hydroxide aqueous solution to the first reactor while stirring, adjust the temperature in the first reactor to 60°C after mixing evenly, react for 30min, and after the reaction is completed, centrifuge and discharge the supernatant to obtain a first mixture.

[0075] Step 3, add 15L copper sulfate mother liquor into the second reactor, the copper ion content of the copper sulfate mother liquor is 70g / L, the pH is 1.50, the calcium content is 263ppm, and the chlorine content is 821ppm. While stirring, add 1kg of the above first mixture into the second reactor, adjust the temperature of the second reactor to 30°C, slowly add 1.5L concentrated sulfuric acid to react for 30min, at this time, the mixed reaction system will release a large number of bubbles, wait until the reaction is completed, after the concentrated sulfuric acid is added, the first mother liquor is obtained. It is dark blue and transparent, the temperature is 62°C, and the copper ion concentration is 158g / L.

[0076] Step 4, the first mother liquor is transferred to an ultrasonic atomization powder making device, the device parameters are adjusted, the ultrasonic frequency is 2.2MHz, an aerosol is formed, the flow rate of carrier gas a is adjusted to 350sccm, the flow rate of carrier gas b is set to 30sccm, the aerosol is taken out by carrier gas a, and protected by carrier gas b, after passing through a 65°C heating device, copper sulfate pentahydrate is generated in situ on a 30°C micro-heated glass substrate, and the product is collected to obtain electroplating grade copper sulfate pentahydrate. The direct yield of the obtained product reaches 85.4%.

[0077] The electroplating grade copper sulfate pentahydrate prepared in this embodiment was tested for metal impurities and chloride ion content. The metal impurities were detected by ICP-OES method with a detection limit of 0.0003%; the chloride ion content was detected by UV-Vis method with a detection limit of 0.001%. The specific test results are shown in Table 3 below:

[0078] Table 3

[0079]

[0080] Figure 3 This is the particle size distribution diagram of the electroplating grade copper sulfate pentahydrate prepared in Example 3. Figure 3 It can be seen that the electroplating-grade copper sulfate pentahydrate prepared in this embodiment has a uniform particle size distribution, and the average particle size is 3.61 μm.

[0081] Example 4

[0082] Step 1, take 5kg of industrial-grade basic copper carbonate with an iron content of 200ppm and a copper content of 57%, add 5kg of pure water, stir continuously at a speed of 400rpm / min for 30min, centrifuge, discharge the upper solution to obtain washed basic copper carbonate, dissolve excess copper acetate in water to form a copper ion saturated solution, add acetic acid dropwise to adjust the saturated solution pH to 4.7, add 1.25kg of washed basic copper carbonate to 2.5kg of copper ion saturated solution, centrifuge at 1800rmp / min for 30min, separate, discharge the upper solution, and obtain refined basic copper carbonate. The copper content in the refined basic copper carbonate is 63%.

[0083] Step 2, add 25L 2mol / L glucose aqueous solution to the first reactor, disperse 1.2kg refined basic copper carbonate into 13L pure water and add to the first reactor and stir evenly at 300rmp / min, add 6.5L 7.5mol / L sodium hydroxide aqueous solution to the first reactor while stirring, adjust the temperature in the first reactor to 60°C after mixing evenly, react for 30min, and after the reaction is completed, centrifuge and discharge the supernatant to obtain a first mixture.

[0084] Step 3, add 38L copper sulfate mother liquor into the second reactor, the copper ion content of the copper sulfate mother liquor is 70g / L, the pH is 1.50, the calcium content is 263ppm, and the chlorine content is 821ppm. While stirring, add 2.5kg of the above first mixture into the second reactor, adjust the temperature of the second reactor to 30°C, slowly add 3.8L concentrated sulfuric acid to react for 30min, at this time, the mixed reaction system will release a large number of bubbles, wait until the reaction is completed, after the concentrated sulfuric acid is added, the first mother liquor is obtained. It is dark blue and transparent, the temperature is 62°C, and the copper ion concentration is 155g / L.

[0085] Step 4, the first mother liquor is transferred to an ultrasonic atomization powder making device, the device parameters are adjusted, the ultrasonic frequency is 1.7MHz, aerosol is formed, the flow rate of carrier gas a (air) is adjusted to 400sccm, the flow rate of carrier gas b (air) is set to 35sccm, the aerosol is taken out by carrier gas a, protected by carrier gas b, and then passed through a 65°C heating device to generate copper sulfate pentahydrate in situ on a 35°C micro-heated quartz substrate, and the product is collected to obtain electroplating grade copper sulfate pentahydrate. The direct yield of the obtained product reaches 84.9%.

[0086] The electroplating grade copper sulfate pentahydrate prepared in this embodiment was tested for metal impurities and chloride ion content. The metal impurities were detected by ICP-OES method with a detection limit of 0.0003%; the chloride ion content was detected by UV-Vis method with a detection limit of 0.001%. The specific test results are shown in Table 4 below:

[0087] Table 4

[0088]

[0089] It should be noted that, in this application, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0090] The above-mentioned embodiments are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. A method for preparing electroplating grade copper sulfate pentahydrate using aerosol technology, characterized in that: The following steps are involved: Mixing industrial-grade basic copper carbonate with water and stirring, and then discharging the upper solution to obtain water-washed basic copper carbonate; adding the washed basic copper carbonate to a copper ion saturated solution, centrifuging and discharging the upper layer solution to obtain refined basic copper carbonate; The refined basic copper carbonate and the glucose aqueous solution are mixed evenly, then an alkali solution is added to react, and the supernatant is discharged to obtain a first mixture; The first mixture is mixed with copper sulfate mother liquor, and concentrated acid is added to react to obtain a first mother liquor; The first mother liquid is prepared into an aerosol; the aerosol is carried out by a carrier gas and then heated to generate the electroplating grade copper sulfate pentahydrate in situ on a substrate.

2. The method for preparing electroplating grade copper sulfate pentahydrate by aerosol technology according to claim 1, characterized in that: The pH of the copper ion saturated solution is 0-5; the copper ion saturated solution is a copper salt saturated solution.

3. The method for preparing electroplating grade copper sulfate pentahydrate by aerosol technology according to claim 1, characterized in that: The mass ratio of the water-washed basic copper carbonate to the copper ion saturated solution is (0.5-2):

1.

4. The method for preparing electroplating grade copper sulfate pentahydrate by aerosol technology according to claim 1, characterized in that: The refined basic copper carbonate also includes the step of dispersing the refined basic copper carbonate into water before mixing with the glucose aqueous solution; the mass volume ratio of the refined basic copper carbonate to water is 1g:(2-10)ml; the concentration of the glucose aqueous solution is 2mol / L; the molar mass ratio of glucose in the glucose aqueous solution to the refined basic copper carbonate is 1mol:(20-120)g; the alkaline solution is a sodium hydroxide aqueous solution with a concentration of 7.5mol / L; the volume ratio of the glucose aqueous solution to the alkaline solution is (3-5):

1.

5. The method for preparing electroplating grade copper sulfate pentahydrate by aerosol technology according to claim 1, characterized in that: The copper sulfate mother liquor has a copper ion content of 60-90 g / L and a pH of 0-3.

6. The method for preparing electroplating grade copper sulfate pentahydrate by aerosol technology according to claim 1, characterized in that: The mass ratio of the copper sulfate mother liquor to the first mixture is 1.5L:100g; the concentrated acid is concentrated sulfuric acid; the mass volume ratio of the first mixture to the concentrated acid is 10g:(13-17)ml.

7. The method for preparing electroplating grade copper sulfate pentahydrate by aerosol technology according to claim 1, characterized in that: The first mother liquid is prepared into an aerosol by an ultrasonic atomization powder making device.

8. The method for preparing electroplating grade copper sulfate pentahydrate by aerosol technology according to claim 1, characterized in that: The carrier gas includes carrier gas a and carrier gas b; the carrier gas a is air; the carrier gas b is air; the flow rate of the carrier gas a is 200-500 sccm; the flow rate of the carrier gas b is 20-50 sccm; the heating temperature is 55-70°C.

9. An electroplating grade copper sulfate pentahydrate prepared according to the method according to any one of claims 1 to 8.

10. Use of the electroplating-grade copper sulfate pentahydrate as claimed in claim 9 in electroplating.

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