Reaction tower kettle for efficiently preparing high-purity basic cupric carbonate in large scale in energy-saving manner and use method of reaction tower kettle

Abstract

The invention belongs to the technical field of copper production equipment, and particularly relates to a reaction tower kettle for efficiently preparing high-purity basic cupric carbonate in a large scale in an energy-saving manner. A reaction tower kettle for efficient and energy-saving large-scale preparation of high-purity basic cupric carbonate comprises a stripping tower and a reaction kettle, a plurality of layers of tower plates are arranged in the stripping tower, a gas outlet is formed in the top of the stripping tower, a material distribution disc is arranged below the gas outlet, a gas sensor is arranged between the material distribution disc and the gas outlet, and the gas sensor is connected with the reaction kettle. A material inlet is formed in the side surface of the material distribution disc, and an eccentric stirrer is arranged in the reaction kettle. The device is compact in structure and high in practicability, steam passes through the tower plates layer by layer through combined use of the stripping tower and the reaction kettle, ammonia-containing water vapor can be condensed into water on the tower plates and returns to the reaction kettle with heat, the heated tower plates can heat newly added ammonia water and carbon dioxide, and the heat can be fully utilized.

Description

Technical Field

[0001] The invention belongs to the technical field of copper production equipment, and specifically relates to a reaction tower kettle for efficiently and energy-saving large-scale preparation of high-purity basic copper carbonate and a use method thereof. Background Art

[0002] At present, the production process of metal compounds including nickel carbonate, zinc carbonate, (active) copper oxide, copper carbonate, etc. is long, energy-intensive, the equipment structure is complex, and there are various shortcomings in the process.

[0003] Active copper oxide has the characteristics of high purity, small particle size, large specific surface area, and fast dissolution in the acid specified by the electroplating industry. It has many special properties and great potential application value in the fields of electronics and catalysis. Usually, the carbonate calcination method is mainly used to produce high-purity active copper oxide powder. Due to the long process flow of the carbonate calcination method, the subsequent washing is difficult, the product purity is not high, the dispersibility is not good, and the product activity is not high due to the coarsening of the grains after calcination. The cost is relatively high and high-salt wastewater is generated.

[0004] Regarding the production process of active copper oxide, among some of the currently disclosed invention patents, there are mainly the following commonly used processes: The Chinese patent application number 201127175.2 discloses a process of using copper sulfate and copper material as raw materials, oxidizing them at a low temperature of 80-85°C to obtain copper sulfate crystals, then preparing a solution to react with sodium hydroxide, and then ball milling, filter pressing, washing, drying, and crushing to obtain active copper oxide.

[0005] However, the current solution still has the disadvantages of complex process flow, low degree of integration, large footprint, high energy consumption, and generation of large amounts of wastewater and waste gas. Summary of the invention

[0006] The purpose of the present invention is to provide a reaction tower kettle for preparing high-purity basic copper carbonate on a large scale with high efficiency and energy saving in order to solve the above problems, thereby solving the problems mentioned in the background technology.

[0007] In order to solve the above problems, the present invention provides a technical solution: A reaction tower kettle for efficiently and energy-savingly preparing high-purity basic copper carbonate on a large scale comprises a stripping tower and a reactor, wherein the stripping tower is provided with a plurality of tower plates, a gas outlet is provided at the top of the stripping tower, a distribution disk is provided below the gas outlet, a gas sensor is provided between the distribution disk and the gas outlet, a material inlet is provided on the side of the distribution disk, and an eccentric agitator is provided in the reactor.

[0008] Preferably, a heating jacket is provided on the outside of the reactor, and an electric heating tube is fixedly installed in the jacket.

[0009] Preferably, the stripping tower is provided with an observation window.

[0010] Preferably, a plurality of baffle plates are arranged in the tower plate, gaps are left between the baffle plates, and the baffle plates include a left plate and a right plate, and an angle of 90-140 degrees is formed between the left plate and the right plate.

[0011] Preferably, a circulation pump is provided at the bottom of the reactor.

[0012] Preferably, the heat exchange tubes are made of copper-aluminum alloy.

[0013] Preferably, a temperature sensor is provided in the reactor.

[0014] A method for using a reaction tower kettle for preparing high-purity basic copper carbonate on a large scale with high efficiency and energy saving, comprising the following steps: 1. Add liquid containing copper ammonia into the reactor, preheat it to a certain temperature, and then enter the stripping deammonification tower to pyrolyze and remove the complex between ammonia and copper ions. Condensate at the top of the stripping tower to obtain a mixture of ammonia water and ammonium bicarbonate. Add a certain concentration of ammonia water to supplement the lost ammonia, introduce carbon dioxide to carbonize part of the ammonia, keep the mass concentration of ammonia and ammonium bicarbonate unchanged, and circulate the deammonification leaching reactor.

[0015] 2. The slurry containing basic copper carbonate precipitate is obtained in the bottom of the tower. After filtering, washing and drying, the dried material is crushed, sieved through 100 mesh, analyzed, weighed and packaged to obtain high-purity basic copper carbonate. The basic copper carbonate is roasted to obtain high-purity active copper oxide.

[0016] 3. Pump carbonized ammonia water into the copper bath, add 18t~20t of electrolytic copper as the bottom when slotting, and replenish once a day according to the consumption calculated by output, add a certain amount of ammonium bicarbonate according to the ratio, so that the carbonate content is controlled at 100-110g / L, and cover the charging cover. After about 2 hours of air reaction, pump it into the outer coil to heat the copper bath at 50-70℃, and then react for 2 hours to sample and analyze the copper (Cu) content. The standard is that when Cu is greater than 85g / L, the end point is reached (the time range is 5-12h), close the valve, stop blowing, and copper is finished.

[0017] 4. Ammonia evaporation: Open the reactor inlet valve, open the copper pool filter pump, pump the solution completely into the reactor, and close the inlet valve and filter pump. Turn on the induced draft fan, turn on the automatic switch of the absorption system, and open the relevant valves. Turn on the blower and induced draft fan, turn off the blower after cooling for 1 hour, heat up, control the temperature at 80-100℃, and take samples after about 2 hours until the sample solution is clearly layered, the solution becomes colorless and odorless, and the copper content is ≦0.05g / L, and the reaction is terminated.

[0018] 5. Drying: The material is automatically added to the fully automatic centrifuge through the intermediate stirring tank. The speed of the centrifuge is controlled by PLC. After the material is added, the speed is increased. After 3 minutes, the speed reaches 50Hz and then ends. After the product is dried, the centrifuge automatically unloads the material, puts it into a ton bag, and then adds it to the flash dryer. The inlet air temperature is controlled at 200-260℃, and the outlet air temperature is not lower than 50℃. The material is added and dried.

[0019] The beneficial effects of the present invention are: 1. The present invention has a compact structure and strong practicality. By using the stripping tower and the reactor in combination, steam passes through layers of tower plates, and ammonia-containing water vapor can condense into water on the tower plates and return to the reactor with heat. The heated tower plates can heat newly added ammonia water and carbon dioxide, and can make full use of heat.

[0020] 2. A mixed gas containing ammonium bicarbonate, water and ammonia enters the tower. After cooling, the ammonium bicarbonate is introduced into the stripping tower again, avoiding energy loss caused by direct steam discharge and greatly reducing costs.

[0021] 3. In the process of steaming ammonia, there is no need to introduce steam from the outside for heating, which reduces the overall energy consumption of the stripping tower. In addition, through the above-mentioned waste heat utilization mechanism, the discharged steam can also be used to heat the newly added raw materials, thereby greatly improving the energy utilization rate of the equipment and facilitating practical use. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 It is a schematic diagram of the internal structure of the tower plate of the present invention. DETAILED DESCRIPTION

[0025] like Figure 1-2 As shown, this specific implementation adopts the following technical solutions: Example 1.

[0026] A reaction tower kettle for preparing high-purity basic copper carbonate on a large scale with high efficiency and energy saving, comprising a stripping tower 1 and a reactor 2, wherein the stripping tower 1 is provided with a plurality of trays 3, the top of the stripping tower 1 is provided with a gas outlet 4, a distribution tray 5 is provided below the gas outlet 4, a gas sensor 6 is provided between the distribution tray 5 and the gas outlet 4, a feed inlet 7 is provided on the side of the distribution tray 5, and an eccentric stirrer 8 is provided in the reactor 2. A heating jacket 9 is provided on the outside of the reactor 2, and an electric heating tube 10 is fixedly installed in the heating jacket. An observation window 11 is provided on the stripping tower 1. A plurality of baffles 12 are provided in the tray 3, and gaps are left between the baffles 12. The baffles 12 include a left plate 13 and a right plate 14, and the left plate 13 and the right plate 14 form an angle of 120 degrees. A circulating pump 15 is provided at the bottom of the reactor 2. The heat exchange tubes are all made of copper-aluminum alloy. The present invention adopts a circulating pump structure to add the reaction liquid discharged along with the basic copper carbonate back into the tower kettle.

[0027] A method for using a reaction tower kettle for preparing high-purity basic copper carbonate on a large scale with high efficiency and energy saving, comprising the following steps: 1. Add liquid containing copper ammonia into the reactor 2, preheat it to a certain temperature, and then enter the stripping deammonification tower to pyrolyze and remove the complex of ammonia and copper ions. Condensate at the top of the stripping tower 1 to obtain a mixture of ammonia water and ammonium bicarbonate. Add ammonia water of a certain concentration to supplement the lost ammonia, introduce carbon dioxide to carbonize part of the ammonia, keep the mass concentration of ammonia and ammonium bicarbonate unchanged, and circulate the deammonification leaching reactor.

[0028] 2. The slurry containing basic copper carbonate precipitate is obtained in the bottom of the tower. After filtering, washing and drying, the dried material is crushed, sieved through 100 mesh, analyzed, weighed and packaged to obtain high-purity basic copper carbonate. The basic copper carbonate is roasted to obtain high-purity active copper oxide.

[0029] 3. Pump carbonized ammonia water into the copper bath, add 18t~20t of electrolytic copper as the bottom when slotting, and replenish once a day according to the consumption calculated by output, add a certain amount of ammonium bicarbonate according to the ratio, so that the carbonate content is controlled at 100-110g / L, and cover the charging cover. After about 2 hours of air reaction, pump it into the outer coil to heat the copper bath at 50-70℃, and then react for 2 hours to sample and analyze the copper (Cu) content. The standard is that when Cu is greater than 85g / L, the end point is reached (the time range is 5-12h), close the valve, stop blowing, and copper is finished.

[0030] 4. Ammonia evaporation: Open the inlet valve of reactor 2, open the filter press pump of the copper bath, pump the solution completely into reactor 2, and close the inlet valve and filter press pump. Turn on the induced draft fan, turn on the automatic switch of the absorption system, and open the relevant valves. Turn on the blower and induced draft fan, turn off the blower after cooling for 1 hour, heat up, control the temperature at 80-100℃, and take samples after about 2 hours until the sample solution is clearly layered, the solution becomes colorless and odorless, and the copper content is ≦0.05g / L, and the reaction is terminated.

[0031] 5. Drying: The material is automatically added to the fully automatic centrifuge through the intermediate stirring tank. The speed of the centrifuge is controlled by PLC. After the material is added, the speed is increased. After 3 minutes, the speed reaches 50Hz and then ends. After the product is dried, the centrifuge automatically unloads the material, puts it into a ton bag, and then adds it to the flash dryer. The inlet air temperature is controlled at 200-260℃, and the outlet air temperature is not lower than 50℃. The material is added and dried.

[0032] The beneficial effects of the present invention are: 1. The present invention has a compact structure and strong practicability, and can be used for large-scale production without interruption at one time. By using the stripping tower and the reactor in combination, steam passes through layers of tower plates, and ammonia-containing water vapor can condense into water on the tower plates and return to the reactor with heat. The heated tower plates can heat newly added ammonia water and carbon dioxide, and can make full use of heat.

[0033] 2. A mixed gas containing ammonium bicarbonate, water and ammonia enters the tower. After cooling, the ammonium bicarbonate is introduced into the stripping tower again, avoiding energy loss caused by direct steam discharge and greatly reducing costs.

[0034] 3. In the process of steaming ammonia, there is no need to introduce steam from the outside for heating, which reduces the overall energy consumption of the stripping tower. In addition, through the above-mentioned waste heat utilization mechanism, the discharged steam can also be used to heat the newly added raw materials, thereby greatly improving the energy utilization rate of the equipment and facilitating practical use.

[0035] Since the biggest cost in the current production process is the cost of using steam, that is, the energy cost, the present invention adopts the above structure and innovatively carries out technical transformation of the tower and the reactor, which has continuous and stable production and can process and produce a large amount of raw materials at one time. At the same time, it has the characteristics of low energy consumption and small amount of waste water and exhaust gas, and has important economic and social benefits.

Claims

1. A reaction tower reactor for preparing high-purity basic copper carbonate on a large scale with high efficiency and energy saving, characterized in that: It comprises a stripping tower and a reactor. The stripping tower is provided with several layers of tower plates. The top of the stripping tower is provided with an air outlet. A distribution disk is provided below the air outlet. A gas sensor is provided between the distribution disk and the air outlet. A feeding port is provided on the side of the distribution disk. An eccentric agitator is provided in the reactor.

2. The reaction tower reactor for preparing high-purity basic copper carbonate in a large scale with high efficiency and energy saving according to claim 1, characterized in that: A heating jacket is arranged outside the reaction kettle, and an electric heating pipe is fixedly installed inside the jacket.

3. The reaction tower reactor for preparing high-purity basic copper carbonate in a large scale with high efficiency and energy saving according to claim 2, characterized in that: The stripping tower is provided with an observation window.

4. The reaction tower reactor for preparing high-purity basic copper carbonate in a large scale with high efficiency and energy saving according to claim 3, characterized in that: A plurality of baffles are arranged in the tower plate, gaps are left between the baffles, the baffles include a left plate and a right plate, and an angle of 90-140 degrees is formed between the left plate and the right plate.

5. The reaction tower reactor for preparing high-purity basic copper carbonate in a large scale with high efficiency and energy saving according to claim 4, characterized in that: A circulating pump is arranged at the bottom of the reaction kettle.

6. The reaction tower reactor for preparing high-purity basic copper carbonate in a large scale with high efficiency and energy saving according to claim 5, characterized in that: The heat exchange tubes are all made of copper-aluminum alloy.

7. The reaction tower reactor for preparing high-purity basic copper carbonate in a large scale with high efficiency and energy saving according to claim 6, characterized in that: A temperature sensor is arranged in the reactor.

8. A method for using a reaction tower kettle for preparing high-purity basic copper carbonate in a large scale with high efficiency and energy saving according to any one of claims 1 to 7, comprising the following steps: Add a liquid containing copper ammonia into the reactor, preheat it to a certain temperature, enter the stripping deammonification tower, and then pyrolyze to remove the complex of ammonia and copper ions. Condensate the mixture of ammonia water and ammonium bicarbonate at the top of the stripping tower. Add ammonia water of a certain concentration to supplement the lost ammonia. After carbon dioxide is introduced, part of the ammonia is carbonized to keep the mass concentration of ammonia and ammonium bicarbonate unchanged, and circulate the deammonification leaching reactor. The bottom of the tower obtains a slurry containing basic copper carbonate precipitate, which is filtered, washed and dried, and the dried material is crushed, sieved through 100 meshes, analyzed, weighed and packaged to obtain high-purity basic copper carbonate, and the basic copper carbonate is roasted to obtain high-purity active copper oxide; Pump carbonized ammonia water into the copper bath, add 18t~20t of electrolytic copper as the bottom when slotting, and replenish it once a day according to the consumption calculated according to the output. Add a certain amount of ammonium bicarbonate according to the ratio so that the carbonate content is controlled at 100-110g / L, and cover the feed cover; After about 2 hours of air blowing reaction, it is then pumped into the outer coil heating copper bath at a temperature of 50-70°C. After another 2 hours of reaction, samples are taken to analyze the copper (Cu) content. The standard is that when Cu is greater than 85g / L, the end point is reached (the time range is 5-12h), the valve is closed, the air blowing is stopped, and the copper melting is completed; Ammonia evaporation: open the liquid inlet valve of the reactor, start the filter press pump of the copper bath, pump the solution completely into the reactor, and close the liquid inlet valve and filter press pump; Turn on the induced draft fan, turn on the automatic switch of the absorption system, and open the relevant valves; Turn on the blower and exhaust fan, turn off the blower after cooling for 1 hour, heat up, and control the temperature at 80-100°C. Take samples after about 2 hours until the sample solution is clearly layered, the solution becomes colorless and odorless, and the copper content is ≤0.05g / L, and the reaction is terminated; Drying: The material is automatically added to the fully automatic centrifuge through the intermediate stirring tank. The speed of the centrifuge is controlled by PLC. After the addition is completed, the speed is increased and the process ends after 3 minutes when the speed reaches 50Hz. After the product is dried, the centrifuge automatically unloads the material, puts it into a ton bag, and then adds it to the flash dryer. The inlet air temperature is controlled at 200-260℃, the outlet air temperature is not lower than 50℃, and the material is added for drying.

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