Spherical basic copper chloride and a method for producing the same

Abstract

This application provides a spherical basic copper chloride and its preparation method. The preparation method includes: mixing seed crystals and water uniformly to obtain a seed crystal dispersion; the seed crystals include hydrochloric acid-catalyzed basic copper chloride; adding purified acidic copper-containing etching waste liquid, ammonia, and a stabilizer to the seed crystal dispersion to obtain a mixed reactant with a pH value of 4-5.5; heating the mixed reactant at a temperature of 40-80°C and stirring at a stirring speed of 100-200 r / min; separating the reactants after the reaction, collecting the solid material, and drying it to obtain the spherical basic copper chloride. In this application, during the crystal growth process, the reaction temperature is controlled to control the growth rate of the seed crystals, and the stirring speed is controlled to control the morphology of the crystals, thereby controlling the growth of the crystals to obtain spherical basic copper chloride. Furthermore, the continuous stirring process grinds the crystal surface, strengthening the structural strength of the crystals, resulting in a final crystal with a smooth surface and good overall structural stability.

Description

Technical Field

[0001] This application relates to the preparation of basic copper chloride, and more particularly to a spherical basic copper chloride and a method for its preparation. Background Technology

[0002] Basic copper chloride, also known as copper oxychloride or royal copper, has the molecular formula Cu2(OH)3Cl. It appears as green or dark green crystalline powder, insoluble in water but soluble in dilute acids and ammonia. Because basic copper chloride is insoluble in water yet dissolves rapidly and readily in the animal's intestines, it has a high utilization rate compared to other copper sources. It is stable, has low hygroscopicity, and does not accelerate the oxidation of vitamins and antibiotics. Therefore, it has been widely used as a copper-based feed additive in recent years.

[0003] Currently, the method for producing basic copper chloride involves reacting copper-containing wastewater with ammonia water under specific reaction conditions. However, the basic copper chloride produced by this method suffers from poor structural stability. Summary of the Invention

[0004] In view of this, this application provides a spherical basic copper chloride and a method for preparing the same.

[0005] To achieve the above objectives, this application provides a method for preparing spherical basic copper chloride. The method includes: mixing seed crystals and water uniformly to obtain a seed crystal dispersion, wherein the seed crystals include hydrochloric acid-catalyzed basic copper chloride; adding purified acidic copper-containing etching waste liquid, ammonia, and a stabilizer to the seed crystal dispersion to obtain a mixed reactant with a pH value of 4–5.5; heating the mixed reactant at a temperature of 40–80°C and stirring it at a stirring speed of 100–200 r / min; separating the reactants after the reaction, collecting the solid material, and drying it to obtain the spherical basic copper chloride.

[0006] In some possible implementations, the flow rate ratio of the acidic copper-containing etching waste liquid to the ammonia water is 2:1 to 6:1, the concentration of copper ions in the acidic copper-containing etching waste liquid is 80 to 150 g / L, and the mass fraction of the ammonia water is 15 to 30%.

[0007] In some possible implementations, the content of the seed crystals in the mixed reactants is 50–150 kg / m³. 3 .

[0008] In some possible implementations, the stabilizer is ammonium bicarbonate, and the amount of the stabilizer added is 1 / 1000 to 1 / 100 of the total mass of the seed dispersion, the acidic copper-containing etching waste liquid, and the ammonia water.

[0009] In some possible implementations, the reaction time is 2 to 8 hours.

[0010] In some possible implementations, the flow rate of the acidic copper-containing etching waste solution added is 2–3 m / s. 3 / h.

[0011] In some possible implementations, the drying temperature is 50–130°C.

[0012] In some possible implementations, the separation includes hydrocyclone separation, which includes: separating the reacted liquid mixture into solids and suspensions at 30-70 r / min, collecting the solids, and adding the suspensions to the reactants for further reaction.

[0013] In some possible implementations, the growth rate of the spherical basic copper chloride during the reaction is less than 2 μm / h.

[0014] This application also provides a spherical basic copper chloride, prepared according to a preparation method.

[0015] In this application, hydrochloric acid is used as a catalyst for basic copper chloride as a seed crystal. Copper and ammonia react in an acidic copper-containing etching waste liquid, and the reaction product rapidly grows on the seed crystal surface to form crystals. The crystals continuously grow to form spherical basic copper chloride. During the crystal growth process, the reaction temperature is controlled to control the growth rate of the seed crystal, and the stirring speed is controlled to control the morphology of the crystal, thereby controlling the growth of the crystal and transforming its surface from irregular to regular spherical shape, thus obtaining spherical basic copper chloride. Furthermore, the continuous stirring process grinds the crystal surface, strengthening the structural strength of the crystal, resulting in a smooth surface and good overall structural stability and high hardness of the final crystal. The spherical basic copper chloride prepared in this application has a particle size between 50 and 100 μm and a purity of up to 99%. It can be used as a raw material for the production of downstream copper salt products (such as copper hydroxide or copper chloride), as well as a copper source for feed additives and inorganic copper preparations in pesticides (such as copper hydroxide). Meanwhile, the spherical basic copper chloride prepared in this application has a stable structure, is resistant to storage, has good dispersibility, and good structural uniformity. Attached Figure Description

[0016] Figure 1 The image shows the X-ray diffraction pattern of the basic copper chloride product prepared in Example 1 of this application.

[0017] Figure 2 This is a 200x magnified microscope image of the basic copper chloride product prepared in Example 1 of this application.

[0018] Figure 3 This is a microscope image magnified 200 times of the basic copper chloride product prepared in Comparative Example 1 of this application.

[0019] Figure 4 This is a 200x magnified microscope image of the basic copper chloride product prepared in Comparative Example 2 of this application. Detailed Implementation

[0020] Embodiments of the present invention are described in detail below. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.

[0021] In the description of this specification, references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0022] Acidic copper-containing etching waste liquid is the etching waste liquid discharged after etching printed circuit boards (PCBs). It contains a large amount of copper chloride, hydrochloric acid and a small amount of ammonium chloride.

[0023] This application provides a method for preparing spherical basic copper chloride, the method comprising:

[0024] S1. Mix the seed crystals and water evenly to obtain a seed crystal dispersion, wherein the seed crystals include hydrochloric acid-catalyzed basic copper chloride.

[0025] Specifically, this step may involve adding water and seed crystals to a reactor, stirring, and obtaining the seed crystal dispersion. The water should occupy approximately 1 / 5 of the reactor volume, and the mixture should be stirred thoroughly to ensure that the seed crystals are uniformly dispersed in the water.

[0026] Hydrochloric acid-catalyzed basic copper chloride is a product obtained by the chemical catalytic efflorescence of crystalline basic copper chloride with hydrochloric acid, causing the crystalline particles to expand and break apart. Hydrochloric acid-catalyzed basic copper chloride is insoluble in water; therefore, seed crystals are added to water and stirred thoroughly to ensure uniform dispersion, which facilitates subsequent reactions.

[0027] The preparation method of hydrochloric acid-catalyzed basic copper chloride is existing technology, and can be found in patent number 200810218161.2, which will not be elaborated here. In this embodiment, the preparation method of hydrochloric acid-catalyzed basic copper chloride is preferably adopted as described in the above-mentioned patent Example 1. The difference between this embodiment and Example 1 is that the acetic acid in Example 1 is replaced with hydrochloric acid, while other conditions remain unchanged, to obtain the prepared hydrochloric acid-catalyzed efflorescent basic copper chloride product.

[0028] The aforementioned hydrochloric acid-catalyzed basic copper chloride has a rough surface with depressions and small crystal particles. Basic copper chloride crystals exist in various types, and the microstructure and stability of basic copper chloride prepared using different crystal forms as seed crystals differ, and they can also interconvert under certain conditions. The hydrochloric acid-catalyzed basic copper chloride used in this application as a seed crystal facilitates the formation of stable spherical basic copper chloride during subsequent crystal growth, and ensures that the subsequent crystals grow into uniformly sized crystals.

[0029] S2. Add the purified acidic copper-containing etching waste liquid, ammonia, and stabilizer to the seed dispersion to obtain a mixed reactant with a pH of 4 to 5.5.

[0030] In this process, since the acidic copper-containing etching waste liquid is highly acidic, the addition of ammonia can adjust the pH of the reaction, and the reaction can be controlled and kept mild, which is beneficial for treating the wastewater from the subsequent preparation of spherical basic copper chloride in this application. At the same time, ammonia is also added as a reactant, which is inexpensive and readily available. In some embodiments, the pH can be 4, 4.5, 5, or 5.5.

[0031] Acidic copper-containing etching waste liquid refers to the acidic etching waste liquid of printed circuit boards, which contains copper ions and chloride ions. In some embodiments, the acidic copper-containing etching waste liquid after impurity removal refers to the acidic copper-containing etching waste liquid obtained after removing impurities such as dioxins, arsenic, lead, cadmium and insoluble solids.

[0032] The impurity removal step of the acidic copper-containing etching waste liquid is an existing technology. For details, please refer to the records of patent numbers 200810141671.4 and 201010567599.9. It will not be elaborated here.

[0033] S3. Heat the mixed reactants at a temperature of 40-80°C and stir them at a stirring speed of 100-200 r / min. After the reaction, separate the solid material, dry it, and obtain the spherical basic copper chloride.

[0034] The main chemical reaction that occurs in this step is:

[0035] 2CuCl2+3NH3·H2O=Cu2(OH)3Cl+3NH4Cl

[0036] Through the above reaction, Cu2(OH)3Cl is grown on the surface of basic copper chloride seed crystals catalyzed by hydrochloric acid and crystallized to form spherical basic copper chloride.

[0037] Using hydrochloric acid as a catalyst, basic copper chloride is used as a seed crystal. Copper and ammonia react in acidic copper-containing etching waste liquid, and the reaction product rapidly grows on the seed crystal surface to form crystals. The crystals continue to grow, and the overall structure of the crystals is stabilized by a stabilizer to obtain stable spherical basic copper chloride. During the crystal growth process, the reaction temperature is controlled to control the crystal growth rate, and the crystal morphology is controlled by controlling the stirring speed, thereby controlling the crystal growth and transforming the irregular surface of the crystals into regular spherical shapes, thus obtaining spherical basic copper chloride. Furthermore, the continuous stirring process grinds the crystal surface, strengthening the structural strength of the crystals, resulting in a smooth surface and good overall structural stability and high hardness of the final crystals. The spherical basic copper chloride prepared in this application has a particle size between 50 and 100 μm and a purity of up to 99%. It can be used as a raw material for the production of downstream copper salt products (such as copper hydroxide or copper chloride), as well as a copper source for feed additives and inorganic copper preparations in pesticides (such as copper hydroxide). Meanwhile, the spherical basic copper chloride prepared in this application has a stable structure, is resistant to storage, has good dispersibility, and good structural uniformity.

[0038] In the above preparation process, reaction temperature and stirring speed affect the formation of spherical basic copper chloride crystals. The reaction product Cu2(OH)3Cl crystallizes and grows on the seed crystal surface, a process of wear down the irregular surface of the crystal to a regular spherical surface. Under suitable reaction temperature conditions, crystal growth is favorable for forming spherical basic copper chloride. Controlling the stirring speed during crystal growth controls the wear rate on the crystal surface, thus achieving a balance between the crystal growth rate and the wear rate, resulting in smooth-surfaced spherical basic copper chloride. In actual production, if the crystal growth rate is less than the wear rate, the resulting crystal will have an irregular morphology and poor overall structural stability due to insufficient wear on the crystal surface. Therefore, during crystal growth, it is necessary to control the crystal growth rate to ensure it does not exceed the wear rate.

[0039] In this embodiment, the reaction temperature is 40–80°C. If the reaction temperature is too high, such as above 80°C, the crystal growth and aging process will accelerate, increasing the crystal hardness and relatively reducing the wear rate on the crystal surface. If the reaction temperature is too low, such as below 40°C, it will affect the crystal growth rate, making it difficult for the crystal to form a spherical shape. In some embodiments, the reaction temperature can be 40°C, 45°C, 50°C, 55°C, 60°C, 70°C, or 80°C.

[0040] In this embodiment, the stirring speed is 100–200 r / min. If the stirring speed is too low, such as less than 100 r / min, the stirring speed is insufficient, the probability of contact wear between crystals decreases, and the wear rate of the crystals is reduced to a certain extent, eventually leading to the formation of basic copper chloride with other morphologies. If the stirring speed is too high, the wear on the crystal surface is greater, making it more difficult to deposit spherical basic copper chloride of a certain particle size on the crystal surface. In some embodiments, the stirring speed is 100 r / min, 120 r / min, 140 r / min, 150 r / min, 160 r / min, 180 r / min, or 200 r / min.

[0041] In some embodiments, the flow ratio of the acidic copper-containing etching waste liquid to the ammonia solution is 2:1 to 6:1, the concentration of copper ions in the acidic copper-containing etching waste liquid is 80 to 150 g / L, and the mass fraction of the ammonia solution is 15% to 30%. Under the above-mentioned suitable flow ratio, concentration, and mass fraction, the copper in the acidic copper-containing etching waste liquid can be fully reacted with the ammonia solution, and excessive ammonia solution can be avoided. In some embodiments, the flow ratio of the acidic copper-containing etching waste liquid to the ammonia solution is 2:1, 3:1, 4:1, 5:1, or 6:1. The concentration of copper ions is 80 g / L, 90 g / L, 100 g / L, 110 g / L, 120 g / L, or 150 g / L. The mass fraction of the ammonia solution is 15%, 20%, 25%, or 30%.

[0042] In some embodiments, the content of the seed crystals in the mixed reactants is 50–150 kg / m³. 3 Based on the amounts of acidic copper-containing etching waste liquid and ammonia added, within such a range, the reaction products are grown in the seed crystal. In some embodiments, the seed crystal content is 50 kg / m³. 3 60kg / m 3 80kg / m 3 100kg / m 3 120kg / m 3 130kg / m 3 Or 150kg / m 3 In some embodiments, the seed crystals have a particle size of 0.1 μm-50 μm.

[0043] In some embodiments, the flow rate of the acidic copper-containing etching waste solution added is 2–3 m / s. 3 Within this flow rate range, and by correspondingly controlling the flow rate of ammonia water, the acidic copper-containing etching waste liquid and ammonia water can be fully reacted. Simultaneously, this facilitates the integration of the entire preparation reaction process with other reaction conditions such as temperature and stirring rate to control the morphology of the reaction product and avoid uncontrollable product growth due to excessively high flow rates. In some embodiments, the flow rate is 2 m / h. 3 / h, 2.5m3 / h, 2.8m 3 / h or 2m 3 / h.

[0044] In some embodiments, the reaction time is 2–8 hours to maintain a certain crystal growth rate in the reactor. The reaction time is inversely proportional to the concentrations of the acidic basic copper chloride waste liquid and ammonia. Unlike other layered growth methods for basic copper chloride, the crystal growth of spherical basic copper chloride belongs to a diamond-like spherical structure growth method, which places extremely high demands on the crystal growth rate. When the growth rate is too fast, the deposition rate on the crystal surface is too rapid, and the growth method will become a layered growth method, easily forming other crystal forms of basic copper chloride, resulting in irregular morphologies such as serrated edges on the crystal surface. Therefore, it is necessary to control the crystal growth rate by controlling the flow rate of the acidic basic copper chloride waste liquid, the flow rate of the ammonia, and the reaction time.

[0045] In some embodiments, during the reaction process, the growth rate of spherical basic copper chloride is less than 2 μm / h, and the crystal growth rate is controlled to not exceed 2 μm / h, specifically 1.8 μm / h, 1.5 μm / h, 1.3 μm / h, 1 μm / h, or 0.5 μm / h. Preferably, it is 1 μm / h. In the above process, controlling the growth rate to 2 μm / h, based on the seed crystal's experienced particle size as the initial particle size, and the final desired particle size of the spherical basic copper chloride as the target particle size, the growth rate required per hour is calculated using the difference between the target particle size and the initial particle size, thus obtaining the growth rate.

[0046] In some embodiments, the stabilizer is ammonium bicarbonate, and the amount of stabilizer added is 1 / 1000 to 1 / 100 of the total mass of the seed dispersion, acidic copper-containing etching waste liquid, and ammonia. During the preparation process, the stabilizer and water are mixed to prepare a 30% (w / w) solution and added proportionally. The addition of the stabilizer stabilizes the crystal form of spherical basic copper chloride, ultimately yielding stable spherical basic copper chloride. In some embodiments, the amount of stabilizer added can be 1 / 1000, 1 / 800, 1 / 500, 1 / 300, or 1 / 100 of the total mass of the reactants (seed dispersion, acidic copper-containing etching waste liquid, and ammonia).

[0047] The specific method for separation in step S3 is as follows: the product after the reaction of the mixed reactants is transported to a hydrocyclone for separation, the separated solid material is collected, dried, and spherical basic copper chloride is obtained.

[0048] In some embodiments, a hydrocyclone is used for hydrocyclone separation at a rotation speed of 30–70 r / min. Solid and suspended materials are separated, and the suspended material is recovered and added back to the reactor as a mixed reactant, thereby improving the utilization rate of the mixed reactant and saving costs. Hydrocyclone separation technology can screen out basic copper chloride particles that meet the particle size and morphology requirements from the reaction products. Smaller particles of basic copper chloride are mixed in the suspended material; this suspended material is then added back to the mixed reactant to continue the reaction and collect more spherical basic copper chloride. In some embodiments, the rotation speed of the hydrocyclone can be 30 r / min, 40 r / min, 50 r / min, or 70 r / min.

[0049] In some embodiments, the temperature for drying the solid material is 50–130°C to fully dry the solid material, reduce its water content, improve the structural stability of the final product, spherical basic copper chloride, and prevent clumping due to the presence of moisture in the basic copper chloride during subsequent storage. In actual production, the solid material separated from the hydrocyclone is wet, and within the above temperature range, the solid material can be fully dried. The drying temperature can be 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, 120°C, or 130°C.

[0050] This application also provides a spherical basic copper chloride, prepared by the above-described method. The spherical basic copper chloride prepared in this application has a smooth surface, a particle size of 50–100 μm, and a purity of over 99%. The spherical basic copper chloride prepared in this application can be used as a raw material for the production of downstream copper salt products, such as copper hydroxide and copper chloride, as well as as a copper source for feed additives and as a raw material for inorganic copper preparations such as copper oxychloride in the pesticide field. Furthermore, due to the special spherical morphology of the basic copper chloride prepared by this method, it has greater application and development value in materials science and other fields.

[0051] The present invention will be explained below with reference to embodiments. Those skilled in the art will understand that the following examples are for illustrative purposes only and should not be construed as limiting the invention. Unless otherwise stated, reagents, software, and instruments involved in the following embodiments that are not specifically described are all conventional commercially available products or open-source materials.

[0052] The composition of the purified acidic copper-containing etching waste liquid used in this application is shown in Table 1. The following examples and comparative examples all use purified acidic copper-containing etching waste liquid, which refers to the acidic copper-containing etching waste liquid obtained after removing impurities such as dioxins, arsenic, lead, cadmium, nickel, and insoluble solids.

[0053] Table 1. Component content of acidic copper-containing etching wastewater after impurity removal.

[0054] project Cu, g / L H, mol / L Ni, mg / L Cd, mg / L As, mg / L Pb, mg / L Dioxins, ng / kg content 120 1.5 0.5 0.05 0.1 0.04 17

[0055] Example 1

[0056] In a 5 cubic meter reactor, 1 cubic meter of water and 0.5 kg of hydrochloric acid-catalyzed basic copper chloride seed crystals were added and stirred thoroughly to obtain a seed crystal dispersion.

[0057] With 2m 3 The flow rate of / h will be 2m 3 The above-mentioned acidic copper-containing etching waste liquid was treated at a concentration of 0.5 m... 3 The flow rate will be 0.5m / h. 3 Ammonia solution with a mass fraction of 20% and ammonium bicarbonate stabilizer (5.8 kg / h) were simultaneously added to the reactor and mixed with the seed crystal dispersion to obtain a mixed reactant with a pH of 4.8. The mixed reactant was heated and continuously stirred at a stirring speed of 180 r / min at a temperature of 45°C for 5 h. After that, the reaction product was transferred to a hydrocyclone for hydrocyclone separation at a rotation speed of 50 r / min, separating the solid material and the suspended material. The suspended material was added back to the reactor for re-reaction. The collected solid material was dried at 70°C for 5 h to obtain 198 g of spherical basic copper chloride product.

[0058] Comparative Example 1

[0059] The difference between Comparative Example 1 and Example 1 is that the seed crystal used in Comparative Example 1 is the product of basic copper chloride catalytic weathering by acetic acid (the specific preparation steps are described in Example 1 of Patent No. 200810218161.2), and the other steps are the same as in Example 1.

[0060] Comparative Example 2

[0061] The difference between Comparative Example 2 and Example 1 is that no seed crystals or stabilizers were added to the reactor; the other steps were the same as in Example 1. See also... Figure 1 The product prepared in Example 1 was subjected to X-ray diffraction testing. The analytical instrument used was an X-ray diffractometer (SHIMADZU XRD~6000, D / max 2500V / pc, Cu Kαradiation), with continuous scanning mode, scanning range 10~75deg, scanning speed 5deg / min, presentation time 1.00sec, voltage 40kV, and current 30A. Figure 1As can be seen from the XRD pattern, the product obtained in Example 1 has a good match with the XRD pattern on card 78-0372 (Cu2Cl(OH)3, Atacamite). This product belongs to the orthorhombic Pnma(62) crystal system with a cell parameter of 6.03×6.865×9.12 (90.0×90.0×90.0). This indicates that the product prepared in this application is a basic copper chloride product.

[0062] This application also includes microscopic testing of the product prepared in Example 1 at 200x magnification. The analytical instrument was a metallurgical microscope (analytical instrument: Leica DM2500M, Germany). From Figure 2 As can be seen, the product crystals are dark green spherical with smooth surfaces and uniform particle size. This indicates that spherical basic copper chloride was successfully prepared in Example 1.

[0063] In addition, this application also conducted microscopic tests at magnification on the basic copper chloride products prepared in Comparative Example 1 and Comparative Example 2. From Figure 3 As can be seen, the surface of the basic copper chloride product has many sharp edges and corners, is irregular, and does not form spherical particles. This indicates that in Example 1, when hydrochloric acid was used as a seed crystal to catalyze basic copper chloride, the chloride ions in the hydrochloric acid act on the basic copper chloride during the preparation process, which is beneficial for the subsequent formation of spherical basic copper chloride.

[0064] from Figure 4 Observation revealed that even without the addition of seed crystals and stabilizers, basic copper chloride exhibited numerous sharp edges and corners on its surface, with uneven particle size and irregular shapes. This indicates that the combination of seed crystals and stabilizers facilitates the formation of spherical basic copper chloride.

[0065] The above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions to the technical solutions of the present invention should not depart from the spirit and scope of the technical solutions of the present invention.

Claims

1. A process for the preparation of spherical basic copper chloride, characterized in that, The preparation method includes: The seed crystals and water are mixed evenly to obtain a seed crystal dispersion. The seed crystals are hydrochloric acid catalyzed basic copper chloride. The hydrochloric acid catalyzed basic copper chloride is the product obtained after crystalline basic copper chloride undergoes chemical catalytic efflorescence with hydrochloric acid, causing the crystalline particles to expand and break apart. Add impurity-removed acidic copper-containing etching waste liquid, ammonia water, and a stabilizer, wherein the stabilizer is ammonium bicarbonate, to the seed dispersion to obtain a mixed reactant with a pH value of 4 to 5.5; The mixed reactants are heated to a temperature of 40-80°C and stirred at a stirring speed of 100-200 r / min. After the reaction, the mixture is separated, the solid material is collected, and dried to obtain the spherical basic copper chloride. During the reaction, the growth rate of the spherical basic copper chloride is less than 2 μm / h.

2. The method for preparing spherical basic copper chloride according to claim 1, characterized in that, The flow rate ratio of the acidic copper-containing etching waste liquid to the ammonia water is 2:1 to 6:1, the concentration of copper ions in the acidic copper-containing etching waste liquid is 80 to 150 g / L, and the mass fraction of the ammonia water is 15 to 30%.

3. The method for preparing spherical basic copper chloride as described in claim 2, characterized in that, The content of the seed crystal in the mixed reactant is 50-150 kg / m 3 .

4. The method for preparing spherical basic copper chloride as described in claim 1, characterized in that, The amount of stabilizer added is 1 / 1000 to 1 / 100 of the total mass of the seed dispersion, the acidic copper-containing etching waste liquid, and the ammonia water.

5. The method for preparing spherical basic copper chloride as described in claim 1, characterized in that, The reaction time is 2-8 hours.

6. The method for preparing spherical basic copper chloride as described in claim 1, characterized in that, The flow rate of the acidic copper-containing etching waste solution added is 2 to 3 m 3 / h.

7. The method for preparing spherical basic copper chloride as described in claim 1, characterized in that, The drying temperature is 50~130℃.

8. The method for preparing spherical basic copper chloride as described in claim 1, characterized in that, The separation includes hydrocyclone separation, which includes: separating the reacted liquid mixture into solid material and suspended material at 30-70 r / min, collecting the solid material, and adding the suspended material into the mixed reactants for further reaction.

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