Production device of reagent-grade copper sulfate

Abstract

The copper sulfate production device comprises a filter pressing crystallization device, a mother liquor recovery device, a medicine storage tank and a water supply device which are connected in sequence, wherein a centrifugal machine of the filter-press crystallization device is provided with a solid discharge port and a liquid discharge port, the solid discharge port of the centrifugal machine is connected with the fluidized bed dryer, and the liquid discharge port is connected with a mother liquor pool of the mother liquor recovery device; and the mother liquor pool is connected with the recrystallization tank for mother liquor recycling, and is also connected with the evaporation device for recycling electroplating-grade copper sulfate after evaporation crystallization. The device disclosed by the utility model has the advantages of simple and feasible preparation method, low treatment cost, recyclable mother liquor and extremely low product impurity content, reaches the standard (HGT 5725-2020) of high-purity reagent copper sulfate pentahydrate, and improves the product quality of copper sulfate salt.

Description

Technical Field

[0001] The utility model relates to the technical field of copper sulfate production, in particular to a production device for reagent-grade copper sulfate pentahydrate. Background Art

[0002] Copper sulfate is widely used in a wide range of industries. Among them, the main content of electroplating grade copper sulfate pentahydrate is more than 99%, the metal iron ion is lower than the industrial grade, and the chloride content is far lower than the industrial grade, which cannot exceed 0.002%. Copper sulfate is the main material for acid copper plating and is the Cu in the plating solution. 2+ Furthermore, the requirements for high-purity reagent-grade copper sulfate pentahydrate are more stringent, with the main content reaching more than 99.5%, the metallic iron ion less than 0.001%, and the chloride not exceeding 0.0005% (HGT 5725-2020).

[0003] The existing production of copper sulfate pentahydrate generally adopts by-product recovery or acidification treatment of waste copper, and the preparation processes generally include ammonia leaching, catalytic oxidation, extraction, etc. However, for now, the production of copper sulfate pentahydrate is still mainly based on rough processing, mainly producing agricultural and industrial grade copper sulfate. The production of electroplating grade copper sulfate pentahydrate and high-purity reagent grade copper sulfate pentahydrate with higher requirements will use purer raw materials, such as high-purity copper as raw materials. Although this process is simple and has stable quality, it is costly. There is also the production of electroplating grade copper sulfate by industrial copper sulfate recrystallization method, and the product quality is difficult to guarantee, and because of its high heavy metal impurities and chlorine content, it is technically difficult to remove these impurities. Utility Model Content

[0004] In order to overcome the defects of the prior art, the utility model provides a production device for reagent-grade copper sulfate.

[0005] The technical solution of the utility model is: a copper sulfate production device, which comprises: a filter press crystallization device, a mother liquor recovery device, a drug storage tank, and a water supply device.

[0006] Specifically, the filter press crystallization device comprises a crystallization tank, a hot filter press, a recrystallization tank, a centrifuge, and a dryer, and the crystallization tank, the hot filter press, the recrystallization tank, the centrifuge, and the dryer are connected in sequence.

[0007] Specifically, the mother liquor recovery device includes a mother liquor tank and an evaporation device.

[0008] Specifically, the centrifuge is provided with a first discharge port and a second discharge port.

[0009] Specifically, the first discharge port is a solid discharge port, and is connected to the dryer, and the second discharge port is a liquid discharge port, and is connected to the mother liquid pool.

[0010] Specifically, the mother liquor pool is connected to the recrystallization tank and the evaporation device, and the evaporation device is used for reflux of the copper sulfate solution after evaporation and crystallization.

[0011] Specifically, the recrystallization tank is used to remove impurities in the copper sulfate solution.

[0012] Specifically, the temperature of the copper sulfate solution is greater than 80° C., the Baume degree is 1.35 to 1.45, and the pH value is 1.5 to 2.5.

[0013] Specifically, the recrystallization tank is used to add hydrogen peroxide, cuprous oxide and activated carbon powder to remove impurities in the copper sulfate solution.

[0014] Specifically, the medicine storage tank includes a first medicine storage tank and a second medicine storage tank, and the water supply device includes a water tank.

[0015] More specifically, a stirring device is provided in both the recrystallization tank and the crystallization tank.

[0016] More specifically, the recrystallization tank is connected to the hot filter press and is also connected to the first drug storage tank, the second drug storage tank, the tap water tank and the steam pipeline;

[0017] More specifically, the liquid medicine in the first medicine storage tank is liquid alkali, which can be transported to the recrystallization tank 1 to adjust the pH so as to be suitable for impurity removal;

[0018] More specifically, the liquid medicine in the second medicine storage tank is sulfuric acid, and the liquid medicine can be transported to the recrystallization tank 1 to adjust the pH so as to be suitable for impurity removal;

[0019] More specifically, the steam pipeline can transport steam to heat the recrystallization tank 1, thereby promoting the recrystallization process.

[0020] More specifically, the hot filter press only has a liquid discharge port, the liquid discharge port of the hot filter press is connected to the crystallization tank, and the hot filter press has the characteristic of strong heat resistance, and the material temperature does not exceed 100°C.

[0021] More specifically, the centrifuge has a solid discharge port and a liquid discharge port, the solid discharge port of the centrifuge is connected to a fluidized bed dryer, and the liquid discharge port of the centrifuge is connected to a mother liquor pool; the fluidized bed dryer produces high-quality reagent-grade copper sulfate products; the mother liquor pool is connected to a recrystallization tank in addition to being connected to a drying device; the drying device produces high-quality electroplating-grade copper sulfate products.

[0022] The production process of the utility model is as follows: firstly, saturated copper sulfate mother liquor, tap water and electroplating grade copper sulfate are put into a recrystallization tank in proportion, and the steam is heated to 80-90°C and the pH is adjusted to 1.5-2.5; after the electroplating grade copper sulfate in the recrystallization tank is completely dissolved, a small amount of hydrogen peroxide, cuprous oxide and activated carbon are put into the recrystallization tank for impurity removal, wherein the role of hydrogen peroxide is to convert ferrous oxide ions into iron ions, and then hydrolyze them into ferric hydroxide precipitation for removal, the role of cuprous oxide is to react chloride ions to generate cuprous chloride precipitation for removal, and the role of activated carbon powder is to adsorb and precipitate the remaining micro heavy metal impurities; after reacting in the recrystallization tank for 20 to 30 minutes, the high-temperature copper sulfate solution is transferred to a hot filter press for filtration, and the filtrate obtained by filtration is transferred to a crystallization tank; the filtrate in the crystallization tank is cooled and crystallized, and when the temperature reaches 25 to 40°C, the solid-liquid mixture is transferred to a centrifuge; the filtrate obtained from the centrifuge is transferred to a mother liquor pool, and the obtained solid is transferred to a fluidized bed dryer for drying, so as to produce a qualified reagent-grade copper sulfate product; a part of the mother liquor entering the mother liquor pool is refluxed into the recrystallization tank, and the other part is opened to flow into the evaporation device, so as to produce a qualified electroplating-grade copper sulfate product, which is then reused.

[0023] Compared with the prior art, the utility model has the following beneficial effects: the preparation method of recrystallization is simple and easy, the processing cost is low, the mother liquor in the whole process can be recycled, and the product has low impurities. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Attached Figure 1 The utility model is a schematic structural diagram of a production device for reagent-grade copper sulfate.

[0025] Figure numerals: 1. recrystallization tank; 2. hot filter; 3. crystallization tank; 4. centrifuge; 5. mother liquor tank; 6. fluidized bed dryer; 7. evaporation device; 8. first medicine storage tank; 9. second medicine storage tank; 10. tap water tank. DETAILED DESCRIPTION

[0026] The technical solution of the utility model will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0027] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installation", "connection" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0028] In addition, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0029] like Figure 1 As shown, the device for producing reagent-grade copper sulfate of the utility model comprises: a recrystallization tank 1, a hot filter press 2, a crystallization tank 3, a centrifuge 4, a mother liquor pool 5, a fluidized bed dryer 6, an evaporation device 7, a first drug storage tank 8, a second drug storage tank 9 and a tap water tank 10. The recrystallization tank 1, the hot filter press 2, the crystallization tank 3, the centrifuge 4 and the fluidized bed dryer 6 are connected in sequence.

[0030] The recrystallization tank 1 is connected to the hot filter press 2. In addition, the recrystallization tank 1 is also connected to the first drug storage tank 8, the second drug storage tank 9, the tap water tank 10 and the steam pipe. The liquid medicine in the first drug storage tank 8 is liquid alkali, which can be transported to the recrystallization tank 1 to adjust the pH so as to be suitable for the occurrence of impurity removal reaction. The liquid medicine in the second drug storage tank 9 is liquid alkali, which can be transported to the recrystallization tank 1 to adjust the pH so as to be suitable for the occurrence of impurity removal reaction. The tap water tank 10 contains tap water, which can be transported to the recrystallization tank 1 to adjust the solution density. First, the copper sulfate mother liquor in the mother liquor pool 5 is transferred to the recrystallization tank 1, and then the stirring device in the recrystallization tank 1 is turned on, and the electroplating grade copper sulfate is put into the recrystallization tank 1 for stirring, and at the same time, the temperature is raised to 80-90° C. through the steam pipeline. After the copper sulfate crystals are completely dissolved, the solution Baume degree is controlled to be 1.35-1.40 by tap water in the tap water tank 10, and the pH is adjusted to 1.5-2.5 by liquid alkali in the first drug storage tank 8 and sulfuric acid in the second drug storage tank 9. Then, appropriate amounts of hydrogen peroxide, cuprous oxide and activated carbon are added to carry out impurity removal reaction. The role of hydrogen peroxide is to convert ferrous oxide ions into iron ions, and then hydrolyze them into iron hydroxide precipitation for removal, the role of cuprous oxide is to react chloride ions to generate cuprous chloride precipitation for removal, and the role of activated carbon powder is to adsorb and precipitate the remaining trace heavy metal impurities.

[0031] After reacting in the recrystallization tank 1 for 20 to 30 minutes, the high-temperature copper sulfate solution is transferred to the hot filter press 2 for filtration to remove impurities. The filtrate obtained from the hot filter press 2 is then transferred to the crystallization tank 3 for cooling and crystallization. When the temperature drops to 25 to 40°C, the solid-liquid mixture is transferred to the centrifuge 4 for centrifugation. Then, the copper sulfate mother liquor obtained from the liquid discharge port of the centrifuge 4 is transferred to the mother liquor pool 5. On the one hand, the mother liquor pool 5 is connected to the recrystallization tank 1, and the mother liquor can be reused; on the other hand, the mother liquor pool 5 is connected to the evaporation device 7. After the mother liquor is evaporated and concentrated by the evaporation device, an electroplating-grade copper sulfate product can be obtained, which can be reused. The solid copper sulfate obtained from the solid discharge port of the centrifuge 4 is transferred to the fluidized bed dryer 6. The copper sulfate obtained after drying in the fluidized bed dryer 5 is the required reagent-grade copper sulfate pentahydrate.

[0032] Specifically, the process of producing reagent-grade copper sulfate is as follows: first, add about 4 to 5 m 3 The copper sulfate mother liquor is placed in a recrystallization tank, and then 1.5-2.0t of electroplating-grade copper sulfate is added, and the temperature is raised to 80-90°C. After the electroplating-grade copper sulfate is completely dissolved, the pH is adjusted to 1.5-2.5, the Baume degree is adjusted to 1.35-1.45, 5-10kg of hydrogen peroxide, 1-2kg of cuprous oxide and 1-2kg of activated carbon powder are added, and then the reaction is continued for 20-30 minutes. The copper sulfate solution is then filtered through a hot filter press and enters a crystallization tank. After cooling and crystallizing in the crystallization tank to 25-40°C, it is transferred to a centrifuge for centrifugation. The resulting mother liquor enters the mother liquor pool, a part of which can be directly reused in the recrystallization tank, and the other part of the open flow can enter the evaporation device, and the evaporation crystallization obtains the electroplating-grade copper sulfate and reuses it in the recrystallization tank; the resulting solid copper sulfate is dried in a fluidized bed dryer to obtain a qualified reagent-grade copper sulfate product.

[0033] Compared with the prior art, the utility model has the advantages of simple and easy recrystallization preparation method, low processing cost, recyclable mother liquor in the whole process, extremely low impurity content of the product, completely meeting the standard of high-purity reagent copper sulfate pentahydrate (HGT 5725-2020), and greatly improving the product quality of copper sulfate salt.

[0034] The above are only preferred embodiments of the present invention. It should be noted that the above preferred embodiments should not be regarded as limiting the present invention. The protection scope of the present invention should be based on the scope defined by the claims. For ordinary technicians in this technical field, several improvements and modifications can be made without departing from the spirit and scope of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention.

Claims

1. A production device for reagent-grade copper sulfate, characterized in that: include: Filter press crystallization device, mother liquor recovery device, drug storage tank, water supply device.

2. The production device of reagent grade copper sulfate according to claim 1, characterized in that, The filter press crystallization device comprises a crystallization tank, a hot filter press, a recrystallization tank, a centrifuge, and a dryer, wherein the crystallization tank, the hot filter press, the recrystallization tank, the centrifuge, and the dryer are connected in sequence; The mother liquor recovery device comprises a mother liquor pool and an evaporation device.

3. The production device of reagent grade copper sulfate according to claim 2, characterized in that, The centrifuge is provided with a first discharge port and a second discharge port; The first discharge port is a solid discharge port and is connected to the dryer, and the second discharge port is a liquid discharge port and is connected to the mother liquid pool; The dryer produces a copper sulfate product.

4. The production device of reagent grade copper sulfate according to claim 2, characterized in that, The recrystallization tank is communicated with the medicine storage tank, the water supply device, and the steam pipeline.

5. The production device of reagent grade copper sulfate according to claim 2, characterized in that, The mother liquor pool is connected to the recrystallization tank and the evaporation device, and the evaporation device is used for refluxing the copper sulfate solution after evaporation and crystallization.

6. The production device of reagent grade copper sulfate according to claim 2, characterized in that, The recrystallization tank is used to remove impurities in the copper sulfate solution.

7. The production device of reagent grade copper sulfate according to claim 5, characterized in that: The copper sulfate solution has a temperature greater than 80° C., a Baume degree of 1.35 to 1.45, and a pH of 1.5 to 2.

5.

8. The production device of reagent grade copper sulfate according to claim 2, characterized in that, The recrystallization tank is used to add hydrogen peroxide, cuprous oxide and activated carbon powder to remove impurities in the copper sulfate solution.

9. The production device of reagent grade copper sulfate according to claim 1, characterized in that: The medicine storage tank includes a first medicine storage tank and a second medicine storage tank, and the water supply device includes a water tank; The liquid medicine in the first medicine storage tank is liquid alkali, and the liquid medicine in the second medicine storage tank is sulfuric acid.

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