TWI636015B - Device for producing metal compound by ammonia method and production process thereof - Google Patents

Abstract

The invention discloses a device for producing a metal compound by an ammonia method and a production process thereof. The device comprises: a leaching tank, a decomposition sedimentation tank and an absorption device; wherein the discharge port of the leaching tank is connected to the feeding port of the decomposition sedimentation tank through a pipeline provided with a filtering device, and the reaction gas outlet of the leaching tank is connected to the intake air of the absorption device; The outlet of the mixed gas of the decomposition sedimentation tank is connected to the air inlet of the absorption device through a pipeline provided with a condenser. The device for producing a metal compound by the ammonia method and the production process thereof are simple, low energy consumption, and environmental protection.

Description

Device for producing metal compound by ammonia method and production process thereof

The invention belongs to the field of chemical industry, and particularly relates to a device for producing a metal compound by an ammonia method and a production process thereof.

At present, the production process of metal compounds including nickel carbonate, zinc carbonate, (active) copper oxide, copper carbonate, etc. is long, energy-consuming, the structure of the equipment is complicated, and various shortcomings exist in the process.

For example, active copper oxide has the characteristics of high purity, small particle size, large specific surface area, and fast dissolution rate in the acid specified by the electroplating industry. It has many specific properties and great potential application value in the fields of electronics and catalysis. Generally, the production of high-purity active copper oxide powder is mainly carried out by the carbonate calcination method. Due to the long process of the carbonate calcination method, subsequent washing is difficult, the product is not high in purity, the dispersion is not good, and the grains are coarsened after calcination Product activity is not high, the cost is relatively high, and high-salt wastewater is generated.

Regarding the production process of active copper oxide, in the presently disclosed invention patents, there are mainly the following commonly used processes:

(1) Chinese Patent Application No. 01127175.2 discloses using copper sulfate and copper materials as raw materials, and oxidizing at 80-85 ° C to obtain copper sulfate crystals, and then preparing a solution to react with sodium hydroxide. Process for preparing active copper oxide by washing, drying and pulverizing.

(2) Chinese Patent Application No. 200710076208.1 discloses a process for producing copper oxide by steaming ammonia from an alkaline etching waste liquid.

The above methods all have the disadvantages of complicated process, equipment and high energy consumption, and will generate a large amount of washing wastewater, which will cause trouble to subsequent processing.

In order to solve the above technical problems, the present invention provides an environmentally-friendly and energy-saving device for producing metal oxides by an ammonia method and a production process thereof.

The invention provides a device for producing a metal compound by an ammonia method, which comprises: a leaching tank, a decomposition and precipitation tank, and an absorption device; wherein the discharging port of the leaching tank is connected to the feeding port of the decomposition and precipitation tank through a pipeline provided with a filtering device, and the leaching tank The reaction gas outlet is connected to the air inlet of the absorption device, and the mixed gas outlet of the decomposition sedimentation tank is connected to the air inlet of the absorption device through a pipeline provided with a condenser; wherein the leaching tank includes: a leaching tank The shell is provided with a reaction gas outlet at the top and a discharge port at the bottom; a circulation pipe fixed to the inside of the leaching tank shell through a support; an isolation sleeve sleeved outside the circulation pipe, and The support is fixed inside the leaching tank housing; the top of the space formed between the circulation pipe and the isolation sleeve is closed; an open orifice plate is provided, which is fixed to the leaching by the support In the groove shell, the edge of the orifice plate is fixedly attached to the inner wall of the leaching groove shell, the lower end of the isolation sleeve is fixed to the orifice plate, and the lower end of the circulation pipe passes through the opening provided in the orifice plate. Into the perforated plate; a reactive gas inlet, which is arranged outside the leaching tank housing and correspondingly located below the perforated plate; the reacted gas inlet is connected to an air inlet pipe, which passes through the The opening of the pipe wall communicates with the circulation pipe; wherein the space between the leaching tank shell and the isolation sleeve is a metal feeding area, and the metal feeding area is located above the orifice plate and the circulation pipe. Below the upper opening, metal raw materials are filled in the metal feeding area.

As a preferred technical solution, the bottom of the space formed between the circulation pipe of the leaching tank and the isolation sleeve is open, and a plurality of circulation holes are provided at the lower part of the tube wall of the isolation sleeve.

As a preferred technical solution, the plurality of circulation holes of the isolation sleeve of the leaching tank are correspondingly located below one-half of the height of the isolation sleeve.

As a preferred technical solution, a circulation baffle is provided above the upper opening of the circulation pipe of the leaching tank, and the circulation baffle is fixed above the upper opening of the circulation pipe through a support frame.

As a preferred technical solution, a feeding hole is provided below the reaction gas outlet at the top of the leaching tank shell of the leaching tank.

As a preferred technical solution, a cooling jacket is sleeved on the outside of the leaching tank shell.

As a preferred technical solution, the cooling sleeve of the leaching tank is located above the orifice plate and below the upper opening of the circulation pipe, the water inlet of the cooling sleeve is located at the lower part of the cooling sleeve, and the water outlet is located at Cool the upper part of the jacket.

As a preferred technical solution, the leaching tank housing, the circulation pipe, the isolation sleeve and the support are all made of stainless steel.

As a preferred technical solution, the decomposition sedimentation tank includes: a sedimentation tank shell, which includes a top region, an upper connection region, a defoaming region, a lower connection region, a rapid heating region, and a bottom region connected to each other from top to bottom; The top zone is provided with a mixed gas outlet; the upper connection zone is provided with an air inlet and a feeding port; the bottom zone is provided with a discharge port; an open orifice plate is provided in the sedimentation tank shell and is located at the speed correspondingly Below the bottom of the hot zone, the edge of the orifice plate is fixed to the inner wall of the sedimentation tank shell; an air stirring tube is provided inside the sedimentation tank shell, one end is connected to the air inlet, and the other end passes through the orifice plate The opening extends into the bottom area below the orifice plate; the heating coil group is fixed on the orifice plate; wherein the inner diameter of the defoaming area is larger than the inner diameter of the rapid heating area.

As a preferred technical solution, the rapid heating zone of the sedimentation tank shell of the decomposition sedimentation tank is provided with a heat medium inlet and a heat medium outlet, the heat medium inlet is connected to the inlet of the heating coil group, and the heat medium outlet is connected An outlet of the heating coil group.

As a preferred technical solution, the heating coil group of the decomposition sedimentation tank includes a plurality of heating coils connected in series.

As a preferred technical solution, the inner diameter of the defoaming zone of the decomposition sedimentation tank is more than 1.1 times the inner diameter of the rapid heating zone.

As a preferred technical solution, the inner diameter of the defoaming zone of the decomposition sedimentation tank is 1.1 times to 5 times the inner diameter of the rapid heating zone.

As a preferred technical solution, the decomposition sedimentation tank further includes: a first insulation sleeve, which is sleeved outside the position of the sedimentation tank housing where the heating sleeve group is provided, and the heat of the first insulation sleeve The medium inlet is connected to a heat medium outlet provided in the rapid heating zone.

As a preferred technical solution, the decomposition and sedimentation tank further includes: a second insulation sleeve, which is sleeved outside the bottom area, and a heat medium inlet of the second insulation sleeve is connected to the first insulation sleeve Heat medium outlet.

As a preferred technical solution, an observation hole is further provided in the top region of the decomposition sedimentation tank.

As a preferred technical solution, the inner diameter of the defoaming zone of the decomposition and precipitation tank is larger than the inner diameter of the top zone.

As a preferred technical solution, the top region, the defoaming region, and the rapid heating region of the decomposition sedimentation tank are cylindrical, and the upper connection region and the lower connection region of the decomposition sedimentation tank are round-shaped and the bottom region is Conical cylindrical shape; the small-diameter top surface of the upper connection area is connected to the bottom surface of the top area, and the small-diameter top surface of the upper connection area is the same as the cross-section of the top area; the large-diameter bottom surface of the upper connection area is connected The top surface of the defoaming region, the large diameter bottom surface of the upper connection region is the same as the cross section of the defoaming region; the large diameter top surface of the lower connection region is connected to the bottom surface of the defoaming region, and the lower connection region The large-diameter top surface is the same as the cross-section of the defoaming area; the small-diameter bottom surface of the lower connection area is connected to the top surface of the rapid heat area, and the small-diameter bottom surface of the lower connection area is connected to the rapid heat area The cross section of the bottom region is the same; the top surface of the bottom region is connected to the bottom surface of the rapid heating region, and the top surface of the bottom region is the same as the cross section of the rapid heating region.

As a preferred technical solution, the absorption device includes at least one absorption tower, and the absorption tower includes a connected top zone, an absorption zone, and a condensation zone from top to bottom; the top zone is provided with a mixed gas outlet; and the bottom of the absorption zone A funnel-shaped bottom plate is provided, and an edge of the funnel-shaped bottom plate is fixed and fixed to an inner wall of the absorption tower, and an outlet of the funnel-shaped bottom plate communicates with the condensation area; An air inlet above the bottom plate; a first orifice plate and a second orifice plate are provided in the absorption area, the first orifice plate is located above the air inlet and the second orifice plate is located above the first orifice plate, The edges of the first orifice plate and the second orifice plate are fixedly attached to the inner wall of the absorption tower; the absorption zone is provided with an absorption liquid inlet, and the absorption liquid inlet is correspondingly located in the first orifice plate and the second orifice. Between the plates; absorbing materials are stacked on the first and second orifice plates; the condensation zone is provided with a condensation device and an absorbing liquid outlet.

As a preferred technical solution, the absorption device includes a plurality of absorption towers connected in series; a mixed gas outlet in a top region of the absorption tower is connected to an air inlet of another absorption tower.

As a preferred technical solution, the device for producing a metal compound by the ammonia method further includes an ammonium carbonate solution storage tank and a water supply device; the top region of the absorption tower is further provided with a reflux liquid inlet, and the absorption liquid outlet of the absorption tower is connected to the previous one The reflux liquid inlet of the absorption tower, the reflux liquid inlet of the first absorption tower is connected to the ammonium carbonate solution storage tank, and the reflux liquid inlet of the last absorption tower is connected to the water supply device.

As a preferred technical solution, an ammonium carbonate solution storage tank is connected to the leaching tank.

As a preferred technical solution, a mixed gas outlet of the last absorption tower in the absorption device is connected to a pressure regulating device.

Preferably, the pressure regulating device is a roots fan.

Preferably, the absorption device includes more than four absorption towers connected in series.

As a preferred technical solution, the absorption liquid outlet of the absorption tower is connected to the absorption liquid inlet of the absorption tower through a pipeline provided with a lift pump.

As a preferred technical solution, an absorption liquid inlet of the absorption tower is connected to a spray pipe provided in the absorption tower, and the spray pipe is correspondingly located below the second orifice plate.

As a preferred technical solution, the condensation device of the absorption device is a condensation coil group, which includes a plurality of condensation coils connected in series.

As a preferred technical solution, the condensation zone of the absorption tower is provided with a cooling medium inlet and a cooling medium outlet, the cooling medium inlet is connected to the inlet of the condensation device, and the cooling medium outlet is connected to the outlet of the condensation device.

The present invention also provides a production process of the above-mentioned device for producing a metal compound by the ammonia method, which is characterized by including the following steps:

(1) Extraction and complexation reaction: adding metal raw materials to the metal feeding area of the leaching tank, then adding an ammonium carbonate solution to the leaching tank, and drumming the inside of the leaching tank through a reaction gas inlet and a circulation pipe Into the air, the blasted air is fully reacted with the ammonium carbonate solution in the circulation tube, and the escaped gas is condensed through the reaction gas outlet of the leaching tank and enters the absorption device. The solution is pushed out of the circulation tube by the air to contact the metal raw material to complex The reaction, at the same time, the solution also flows into the lower part of the orifice plate through the holes of the orifice plate and the circulation holes provided on the isolation sleeve, and then enters the circulation pipe through the lower opening of the circulation pipe to circulate the reaction until the metal content reaches the standard;

(2) Thermal decomposition reaction: After the metal ammonia complex solution obtained in the leaching tank is filtered, it is added to the decomposition precipitation tank from the feeding port of the decomposition precipitation tank, and is performed by a heating coil group in the decomposition precipitation tank. Heating, blowing in air from the air stirring tube at the same time, stirring the solution in the decomposition and precipitation tank, and the metal compound obtained after the decomposition flows out from the discharge opening of the decomposition and precipitation tank;

(3) Tail gas absorption: the gas generated by the decomposition reaction in the decomposition and precipitation tank is cooled and then enters the absorption device for absorption.

The invention can achieve the following technical effects:

(1) The device and process for producing metal compounds by the ammonia method of the present invention are simple, have low energy consumption, and are environmentally friendly.

(2) The leaching tank of the present invention is provided with a circulation pipe, an isolation sleeve (circulation hole), an orifice plate, and a reaction gas inlet so that a cyclic reaction zone is formed inside the leaching tank, which can improve the reaction efficiency and save energy. The leaching tank uses an isolation sleeve and an orifice plate to separate an independent metal feeding area. High-pressure air flows into the circulation pipe to fully react with the leaching solution. The reaction solution sprayed out of the circulation pipe enters the metal feeding area and descends to fully contact the metal. Complexation reaction, repeated cycles, very fast (metals react with the solution to generate ions, the concentration of metal ions in the solution from 0 to 100g / L only takes about 2 hours).

(3) The air stirring function of the decomposition and precipitation tank of the present invention prevents the generated metal compounds from precipitating, and at the same time, the blasted air takes away a large amount of ammonia gas when it rises, reduces the resistance of ammonia gas volatilization in the liquid, and reduces the ammonia gas solution. Possibility of secondary absorption to form ammonia. At the same time, the first insulation sleeve and the second insulation sleeve ensure the full use of heat.

(4) The absorption tower of the absorption device of the present invention can be operated at normal pressure and low pressure, and the stepwise spray absorption method is adopted, which satisfies the production requirements and environmental requirements well.

The present invention will be further described below with reference to the accompanying drawings and specific embodiments, so that those skilled in the art can better understand the present invention and implement it, but the embodiments are not intended to limit the present invention.

As shown in FIG. 1, a preferred embodiment of the device for producing a metal compound by the ammonia method of the present invention includes: a leaching tank 1, a decomposition and sedimentation tank 3, and an absorption device 5; The pipeline of the device 2 is connected to the feeding port of the decomposition sedimentation tank 3, the reaction gas outlet of the leaching tank 1 is connected to the air inlet of the absorption device 5, and the mixed gas outlet of the decomposition sedimentation tank 3 is connected to the absorption device 5 through a pipeline provided with the condenser 4. Air inlet.

As shown in FIG. 2, the molten metal leaching tank 1 for producing metal compounds by the ammonia method of the present invention includes: a leaching tank shell 10 with a reaction gas outlet 100 on the top and a discharge port 110 on the bottom; It is fixed inside the leaching tank housing 10 through the support member 12; the isolation sleeve 13 is sleeved outside the circulation pipe 11 and is fixed inside the leaching tank housing 10 through the support member 14; among them, the circulation pipe 11 and the insulation sleeve The top of the space formed between the tubes 13 is closed; an open orifice plate 15 is provided, which is fixed in the leaching tank housing 10 through the support 16, and the edge of the orifice plate 15 is fixed to the inner wall of the leaching tank housing 10 in a fixed manner. The lower end of the isolation sleeve 13 is fixed on the orifice plate 15, and the lower end of the circulation pipe 11 extends below the orifice plate 15 through the opening provided in the orifice plate 15; the reaction gas inlet 120 is provided outside the leaching tank housing 10, correspondingly Located under the orifice plate 15, the reaction gas inlet 120 is connected to an air inlet pipe 17, and the air inlet pipe 17 communicates with the circulation pipe 11 through an opening provided in a wall of the circulation pipe 11.

The bottom of the space formed between the circulation tube 11 and the isolation sleeve 13 is open, and a plurality of circulation holes 131 are formed in the lower part of the tube wall of the isolation sleeve 13. The plurality of circulation holes 131 correspond to less than one-half the height of the isolation sleeve 13.

A circulation baffle 18 is provided above the upper opening of the circulation pipe 11, and the circulation baffle 18 is fixed above the upper opening of the circulation pipe 11 through a support frame 19 (the support frame 19 is fixed in a space formed between the circulation pipe 11 and the isolation sleeve 13 Closed top).

The space between the leaching tank shell 10 and the isolation sleeve 13 is a metal feeding area 140. The metal feeding area 140 is located above the orifice plate 15 and below the upper opening of the circulation pipe 11, and metal raw materials are filled in the metal feeding area 140.

A feed hole 150 is provided below the reaction gas outlet 100 on the top of the leaching tank shell 10.

A cooling jacket 130 is sleeved on the outside of the leaching tank housing 10. The cooling sleeve 130 is located above the orifice plate 15 and below the upper opening of the circulation pipe 11. The water inlet 1300 of the cooling sleeve 130 is located at the lower portion of the cooling sleeve 130 and the water outlet 1301 is located at the upper portion of the cooling sleeve 1300.

The leaching tank housing 10, the circulation pipe 11, the isolation sleeve 13, and the supporting members 12, 14, 16 are all made of stainless steel.

As shown in FIG. 3, the decomposition and precipitation tank 3 for producing metal compounds by the ammonia method of the present invention includes:

The sedimentation tank shell 31 includes a top region 310, an upper connection region 311, a defoaming region 312, a lower connection region 313, a rapid heating region 314, and a bottom region 315 interconnected from top to bottom. The top region 310, the defoaming region 312, and the rapid heating region 314 are cylindrical, the upper connection region 311 and the lower connection region 313 are circular-conical, and the bottom region 315 is conical. The inner diameter of the defoaming region 312 is larger than the inner diameter of the fast-heating region 314. Preferably, the inner diameter of the defoaming region 312 is more than 1.1 times the inner diameter of the fast-heating region 314. More preferably, the inner diameter of the defoaming region 312 is The inner diameter of the rapid heating zone 314 is 1.1 times to 5 times (this setting can effectively achieve defoaming and gas-liquid separation). The inner diameter of the defoaming region 312 is larger than the inner diameter of the top region 310. The small diameter top surface of the upper connection area 311 is connected to the bottom surface of the top area 310, and the small diameter top surface of the upper connection area 311 is the same as the cross section of the top area 310; the large diameter bottom surface of the upper connection area 311 is connected to the top surface of the defoaming area 312. The large-diameter bottom surface of the upper connection region 311 is the same as the cross-section of the defoaming region 312; the large-diameter top surface of the lower connection region 313 is connected to the bottom surface of the defoaming region 312; The cross section is the same; the small diameter bottom surface of the lower connection area 313 is connected to the top surface of the rapid heat area 314, and the small diameter bottom surface of the lower connection area 313 is the same as the cross section of the rapid heat area 314; The bottom surface of the bottom region 315 is the same as the cross-section of the rapid heating region 314.

The top area 310 is provided with a mixed gas outlet 3100 and an observation hole 3101; the upper connection area 311 is provided with an air inlet 3110 and a feeding port 3111; and the bottom area 315 is provided with a discharging port 3150.

An orifice plate 32 is provided, which is located in the sedimentation tank housing 31 and is located below the bottom of the rapid heat zone 314. The edge of the orifice plate 32 is fixed to the inner wall of the sedimentation tank housing 31;

The air stirring tube 33 is provided inside the sedimentation tank housing 31, one end is connected to the air inlet 3110, and the other end penetrates the opening of the orifice plate 32 into the bottom region 315 below the orifice plate 32;

The heating coil group 34 includes a plurality of heating coils 340 connected to each other, which are fixed on the orifice plate 32. The rapid heating zone 314 is provided with a heat medium inlet 3140 and a heat medium outlet 3141 and a heat medium inlet 3140. The inlet of the heating coil group 34 is connected, and the heat medium outlet 3141 is connected to the outlet of the heating coil group 34.

The first insulation sleeve 35 is sleeved outside the position of the sedimentation tank shell 31 where the heating sleeve group 34 is provided, and the heat medium inlet 350 of the first insulation sleeve 35 is connected to the heat medium provided in the rapid heating zone 314 Outlet 3141 (not shown).

The second heat insulation sleeve 36 is sleeved outside the bottom area 315. The heat medium inlet 360 of the second heat insulation sleeve 36 is connected to the heat medium outlet 351 provided at the first heat insulation sleeve 35.

As shown in FIGS. 4 and 5, the absorption device 5 for producing a metal compound by the ammonia method of the present invention includes at least one absorption tower 51. In a preferred embodiment of the present invention, the absorption tower 51 is connected in series. In the embodiment, in order to ensure optimal absorption efficiency, it is preferable that four or more absorption towers are connected in series, more preferably 4 to 16, and most preferably 8.

The absorption tower 51 includes a connected top region 510, an absorption region 511, and a condensation region 512 from top to bottom;

The top zone 510 is provided with a mixed gas outlet 5100, which can be connected to the air inlet of another absorption tower, and the mixed gas outlet 5100 of the last absorption tower 51 is connected to a roots fan 52 to adjust the pressure in the absorption tower.

The top zone 510 is provided with a mixed gas outlet 5100, which can be connected to the inlet of the next absorption tower, and the mixed gas outlet 5100 of the last absorption tower is connected to a roots fan 52 to adjust the pressure in the absorption tower. The top zone 510 of the absorption tower 51 is also provided with a reflux liquid inlet 5101. The absorption liquid outlet 5120 of the absorption tower is connected to the reflux liquid inlet 5101 of the previous absorption tower through a pipeline provided with a lift pump, and the reflux liquid inlet 5101 of the first absorption tower. The ammonium carbonate solution storage tank 6 is connected, and the return liquid inlet 5101 of the last absorption tower 51 is connected to the water supply device 7. The absorption liquid outlet 5120 of the absorption tower is connected to the absorption liquid inlet 5114 of the absorption tower through a pipeline provided with a lift pump.

The bottom of the absorption area 511 is provided with a funnel-shaped bottom plate 5110. The edge of the funnel-shaped bottom plate 5110 is fixed to the inner wall of the absorption tower 51. The outlet 51100 of the funnel-shaped bottom plate 5110 communicates with the condensation area 512. The absorption area 511 is provided with a corresponding funnel-shaped bottom plate. An air inlet 5111 above 5110; a first orifice plate 5112 and a second orifice plate 5113 are provided in the absorption region 511. The first orifice plate 5112 is located above the air inlet 5111, and the second orifice plate 5113 is located at the first orifice plate 5112. Above, the edges of the first orifice plate 5112 and the second orifice plate 5113 are fixedly attached to the inner wall of the absorption tower 51; the absorption zone 511 is provided with an absorption liquid inlet 5114, and the absorption liquid inlet 5114 is correspondingly located on the first orifice plate 5112 and the second Between the perforated plates 5113; the first perforated plate 5112 and the second perforated plate 5113 are stacked with an absorbing material (not shown in the figure).

The condensation area 512 is provided with a condensation device and an absorption liquid outlet 5120.

In a preferred embodiment of the present invention, the absorption liquid inlet 5114 is connected to a spray pipe 5115 provided in the absorption tower 51, and the spray pipe 5115 is correspondingly located below the second orifice plate 5113.

In a preferred embodiment of the present invention, the condensing device is a condensing coil group 5121, which includes a plurality of condensing coils 51211 connected in series.

In a preferred embodiment of the present invention, the condensation zone 512 is provided with a cooling medium inlet 5122 and a cooling medium outlet 5123. The cooling medium inlet 5122 is connected to the inlet of the condensation device, and the cooling medium outlet 5123 is connected to the outlet of the condensation device.

With reference to FIG. 1 and FIG. 6, the production process of the device for producing metal compounds by the ammonia method of the present invention includes the following steps:

(1) Extraction and complexation reaction: adding metal raw materials to the metal feed zone 140 of the leaching tank 1, and then adding an ammonium carbonate solution to the leaching tank 1, and passing the reaction gas inlet 120 and the circulation pipe 11 to the inside of the leaching tank Air is blown in. After the blown air has fully reacted with the ammonium carbonate solution in the circulation pipe 11, the escaping gas is condensed through the reaction gas outlet 100 of the leaching tank 1 and enters the absorption device 5. The solution is pushed out of the circulation pipe 11 by the air and communicates with The metal raw material is fully contacted to perform the complexation reaction. At the same time, the solution also flows into the lower part of the orifice plate 15 through the holes of the orifice plate 15 and the circulation holes 131 provided on the isolation sleeve 13, and then enters the circulation pipe 11 through the lower opening of the circulation pipe 11. React until the metal content reaches the standard.

(2) Thermal decomposition reaction: After the metal ammonia complex solution obtained in the leaching tank 1 is filtered, it is added from the feeding port 3111 of the decomposition precipitation tank 3 to the decomposition precipitation tank 3, and is performed by the heating coil group 34 in the decomposition precipitation tank 3 Heating, blowing air from the air stirring tube 33 at the same time, stirring the solution in the decomposition precipitation tank 3 (the metal compound is suspended therein), and the metal compound obtained after the decomposition flows out from the discharge port 3150 of the decomposition precipitation tank 3;

(3) Tail gas absorption: The gas generated by the decomposition reaction in the decomposition and precipitation tank 3 is cooled and enters the absorption device 5 for absorption.

Hereinafter, the present invention will be described by taking the preparation of electronic-grade active copper oxide as an example:

(1) Put the cut copper plate into the metal feeding area 140 through the feeding hole 150, add ammonium carbonate solution, air enters the circulation pipe 11 from the reaction gas inlet 120, and the air entering the circulation pipe 11 and the leachate sucked in by the air are in the circulation pipe. 11 is fully reacted, the reacted leachate is blocked by the circulation baffle 18 into the metal feeding area 140 to dissolve the copper plate, and the copper-dissolved liquid enters the circulation pipe 11 through the holes of the orifice plate 15 and the circulation holes 131 provided in the lower part of the isolation sleeve 13, The reaction is continued until the copper content reaches the standard, and a copper ammonia complex is obtained. The copper-ammonia complex is thermally decomposed to obtain copper oxide. The leaching tank 1 of the present invention isolates an independent metal feeding zone 140 by an isolation sleeve 13 and the circulation pipe 11 realizes the stirring function. At the same time, the reaction raw materials required for dissolving copper are dissolved in the leaching solution in the circulation pipe 11 for improving ammonia. Solubility and dissolution rate of copper in leaching solution.

The reaction equation is as follows: Cu + 2NH4HCO3 + 2NH3 + O2 = Cu (NH3) 4CO3 + 2H2O.

(2) The filtered copper ammonia complex solution enters the decomposition precipitation tank 3 through the feeding port 3111, and the air entering from the air stirring tube 33 is evenly distributed through the orifice plate 32 at the bottom for bubble stirring, and the copper ammonia complex solution In the rapid heating zone 314, it is rapidly heated by the heating coil group 34 (the heating medium in the heating coil group can be steam). When the solution reaches a certain temperature, it is decomposed to produce copper carbonate (or copper oxide) and mixed ammonia gas, copper carbonate Suspend in solution with air agitation. A large amount of foam generated due to the rapid decomposition of ammonia gas is used for defoaming and gas-liquid separation in the defoaming zone 312. The separated mixed ammonia gas is discharged to the condenser through the mixed gas outlet 3100 to be condensed into mixed ammonia water. The stirring function of the air stirring tube 33 of the decomposition and precipitation tank 3 of the present invention prevents the generated metal compound (copper carbonate) from precipitating, and at the same time, the swelled air takes away a large amount of ammonia when it rises, and reduces the resistance of ammonia volatilization in the liquid. To reduce the possibility of ammonia gas being absorbed by the solution to form ammonia water. At the same time, the first heat insulation sleeve 35 and the second heat insulation sleeve 36 ensure the full use of heat.

(3) The gas from the leaching tank 1 enters the absorption device 5, the gas from the decomposition precipitation tank 3 is condensed by the condenser 2, and the mixed ammonia gas that has not been completely condensed enters the absorption tower 51 of the absorption device 5, and passes through the orifice plate (the first hole Plate 5112) is evenly distributed and rises to the lower absorbing material (Lacy ring) storage area, and is absorbed by the water liquid on the surface of the absorbing material stacked in the storage area during the ascent. When the mist is absorbed, the mixed ammonia liquid collected at the bottom of the absorption tower is cooled by the cooling coil 51211, and is continuously absorbed by the pump cycle spray. When the ammonia mixed gas not absorbed by the spray passes through the absorption material stacking area on the second orifice plate 5113 at the top The gas-water separation is realized, and the part of the mixed ammonia gas enters the next absorption tower 51 through the mixed gas outlet 5100, and is gradually absorbed until the ammonia tail gas reaches the standard discharge. Among them, in an absorption device composed of a plurality of absorption towers 51 connected in series, the absorption liquid flowing out of the absorption liquid outlet 5120 can be lifted to the absorption liquid inlet 5114 of the absorption tower 51 as an absorption liquid to absorb ammonia, and the absorption tower 51 The absorption liquid flowing out of the absorption liquid outlet 5120 can be lifted into the previous absorption tower 51 from the reflux liquid inlet 5101 of the previous absorption tower 51 to wet the absorption material and absorb ammonia gas. In order to ensure the absorption efficiency, more than four absorption towers 51 can be set (preferably eight), and the operation process can be adjusted by the roots blower 52 at the outlet of the last absorption tower 51 to adjust the micro positive pressure or micro negative pressure as required. Generally common absorption towers are pressure-operated foam absorption towers, which are not suitable for the process requirements for the production of metal compounds by the ammonia method. The step-by-step spray absorption method adopted by the invention satisfies the production requirements and environmental requirements well.

The embodiments described above are merely preferred embodiments for fully explaining the present invention, and the protection scope of the present invention is not limited thereto. Equivalent substitutions or changes made by those skilled in the art on the basis of the present invention are all within the protection scope of the present invention. The protection scope of the present invention is subject to the claims.

In summary, the device for producing metal compounds by the ammonia method according to the present invention and its production process are indeed practical and creative, and the use of its technical means is also novel and undoubted, and the efficacy and design purpose are indeed in line with each other, which has been called a reasonable progress. To Ming. To this end, an application for an invention patent was filed in accordance with the law, but I would like to ask Jun Bureau for detailed review and to grant the patent as a prayer.

1 ‧‧‧extraction tank

10‧‧‧Extraction tank housing

100‧‧‧Reaction gas outlet

110‧‧‧Unloading port

120‧‧‧Reaction gas inlet

130‧‧‧cooling jacket

1300‧‧‧ water inlet

1301‧‧‧ Outlet

140‧‧‧Metal feeding area

150‧‧‧Feed hole

11‧‧‧Circulation tube

12‧‧‧ support

13‧‧‧Isolation sleeve

131‧‧‧Circle hole

14‧‧‧ support

15‧‧‧ Orifice

16‧‧‧ support

17‧‧‧Air inlet duct

18‧‧‧Circular baffle

19‧‧‧ support frame

2‧‧‧filtration device

3‧‧‧ Decomposition sedimentation tank

31‧‧‧Sedimentation tank shell

310‧‧‧Top Zone

3100‧‧‧Mixed gas outlet

3101‧‧‧observation hole

311‧‧‧up connection area

3110‧‧‧Air inlet

3111‧‧‧Feeding port

312‧‧‧Defoaming area

313‧‧‧ under the connection area

314‧‧‧Speed Hot Zone

3140‧‧‧heat medium inlet

3141‧‧‧Heat medium outlet

315‧‧‧bottom

3150‧‧‧Unloading port

32‧‧‧ Orifice

33‧‧‧Air mixing tube

34‧‧‧Heating Coil Unit

340‧‧‧Heating coil

35‧‧‧The first insulation sleeve

350‧‧‧heat medium inlet

351‧‧‧Heat medium outlet

36‧‧‧Second insulation sleeve

360‧‧‧heat medium inlet

4‧‧‧ condenser

5‧‧‧ Absorption device

51‧‧‧ Absorption Tower

51‧‧‧ Absorption Tower

510‧‧‧Top Zone

5100‧‧‧Mixed gas outlet

5101‧‧‧Return liquid inlet

511‧‧‧ absorption zone

5110‧‧‧ Funnel-shaped bottom plate

51100‧‧‧Export

5111‧‧‧Air inlet

5112‧‧‧The first orifice plate

5113‧‧‧Second Orifice

5114‧‧‧ Absorbent inlet

5115‧‧‧spray pipe

512‧‧‧Condensation zone

5120‧‧‧ Absorbent liquid outlet

5121‧‧‧Condensing coil unit

51211‧‧‧Condensing coil

5122‧‧‧Cooling medium inlet

5123‧‧‧ Cooling medium outlet

52‧‧‧Roots Fan

6‧‧‧ ammonium carbonate storage tank

7‧‧‧ water supply device

FIG. 1 is a schematic structural diagram of an apparatus for producing a metal compound by the ammonia method of the present invention. 2 is a schematic cross-sectional structure diagram of an leaching tank of an apparatus for producing a metal compound by an ammonia method according to the present invention. FIG. 3 is a schematic cross-sectional structure diagram of a decomposition precipitation tank of an apparatus for producing a metal compound by the ammonia method of the present invention. 4 is a schematic cross-sectional structure diagram of an absorption tower of an apparatus for producing a metal compound by an ammonia method according to the present invention. FIG. 5 is a schematic cross-sectional structure of an absorption device of an apparatus for producing a metal compound by the ammonia method of the present invention. FIG. 6 is a schematic flow chart of a process for producing a metal compound by the ammonia method of the present invention.

Claims (29)

A device for producing a metal compound by an ammonia method, comprising: an leaching tank, a decomposition and precipitation tank, and an absorption device; wherein the discharge port of the leaching tank is connected to the feeding port of the decomposition and precipitation tank through a pipeline provided with a filtering device, and the reaction gas outlet of the leaching tank; The air inlet of the absorption device is connected, and the mixed gas outlet of the decomposition sedimentation tank is connected to the air inlet of the absorption device through a pipeline provided with a condenser; wherein the leaching tank comprises: a leaching tank shell, A reaction gas outlet is provided at the top, and a discharge opening is provided at the bottom; a circulation pipe is fixed inside the leaching tank shell through a support member; an isolation sleeve is sleeved outside the circulation pipe and fixed by the support member Inside the leaching tank housing; wherein the top of the space formed between the circulation pipe and the isolation sleeve is closed; an open orifice plate is provided, which is fixed in the leaching tank housing by a support, The edge of the orifice plate is fixedly attached to the inner wall of the leaching tank housing, the lower end of the isolation sleeve is fixed on the orifice plate, and the lower end of the circulation tube projects below the orifice plate through the opening provided in the orifice plate. The reaction gas inlet is disposed outside the shell of the leaching tank and is located below the orifice plate. The reaction gas inlet is connected to an air inlet pipe, and the air inlet pipe is connected with an opening provided in a pipe wall of the circulation pipe. The circulation tube is in communication; wherein the space between the leaching tank shell and the isolation sleeve is a metal feeding area, which is located above the orifice plate and below the upper opening of the circulation tube. A metal raw material is filled in the metal feeding area; wherein the bottom of the space formed between the circulation pipe of the leaching tank and the isolation sleeve is open, and a plurality of circulation holes are provided at the lower part of the tube wall of the isolation sleeve . The apparatus for producing a metal compound by the ammonia method according to claim 1, wherein the plurality of circulation holes of the isolation sleeve of the leaching tank are correspondingly located below one-half of the height of the isolation sleeve. The device for producing a metal compound by the ammonia method according to claim 1, wherein a circulation baffle is provided above the upper opening of the circulation pipe of the leaching tank, and the circulation baffle is fixed to the upper opening of the circulation pipe through a support frame. Up. The device for producing a metal compound by the ammonia method according to claim 1, wherein a feeding hole is provided below a reaction gas outlet at the top of the leaching tank shell of the leaching tank. The apparatus for producing a metal compound by the ammonia method according to claim 1, wherein a cooling jacket is sleeved on the outside of the leaching tank shell. The apparatus for producing a metal compound by the ammonia method according to claim 5, wherein the cooling sleeve of the leaching tank is located above the orifice plate and below the upper opening of the circulation pipe, and the inlet of the cooling sleeve is The water outlet is located at the lower part of the cooling jacket, and the water outlet is located at the upper part of the cooling jacket. The apparatus for producing a metal compound by the ammonia method according to claim 6, wherein the leaching tank shell, the circulation pipe, the isolation sleeve, and the support are all made of stainless steel. The device for producing a metal compound by the ammonia method according to claim 1, wherein the decomposition and precipitation tank comprises: a precipitation tank shell including a top region, an upper connection region, a defoaming region, and a lower region connected to each other from top to bottom Connection zone, rapid heating zone and bottom zone; the top zone is provided with a mixed gas outlet; the upper connection zone is provided with an air inlet and a feeding port; the bottom zone is provided with a discharge port; an orifice plate is provided with an opening, It is located in the sedimentation tank shell correspondingly below the bottom of the rapid heat zone, the edge of the orifice plate is fixed and fixed to the inner wall of the sedimentation tank shell; an air stirring tube is set inside the sedimentation tank shell, and one end is connected to the The other end of the air inlet passes through the opening of the orifice plate and extends into the bottom area below the orifice plate; the heating coil group is fixed on the orifice plate; wherein the inner diameter of the defoaming area is larger than that of the rapid heat area path. The device for producing a metal compound by the ammonia method according to claim 8, wherein the rapid heating zone of the precipitation tank shell of the decomposition precipitation tank is provided with a heat medium inlet and a heat medium outlet, and the heat medium inlet is connected to the heating plate The inlet of the tube group and the outlet of the heat medium are connected to the outlet of the heating coil group. The apparatus for producing a metal compound by the ammonia method according to claim 8 or 9, wherein the heating coil group of the decomposition and precipitation tank comprises a plurality of heating coils connected in series. The device for producing a metal compound by the ammonia method according to claim 8 or 9, wherein an inner diameter of a defoaming zone of the decomposition precipitation tank is 1.1 times or more an inner diameter of a rapid heating zone. The apparatus for producing a metal compound by the ammonia method according to claim 11, wherein an inner diameter of a defoaming zone of the decomposition precipitation tank is 1.1 to 5 times an inner diameter of a rapid heating zone. The device for producing a metal compound by the ammonia method according to claim 8, wherein the decomposition and precipitation tank further comprises: a first insulation sleeve, which is sleeved at a position of the sedimentation tank shell provided with a heating sleeve group On the outside, a heat medium inlet of the first heat insulation sleeve is connected to a heat medium outlet provided in the rapid heating zone. The device for producing a metal compound by the ammonia method according to claim 13, wherein the decomposition and precipitation tank further comprises: a second heat insulation sleeve, which is sleeved outside the bottom area, and the heat medium of the second heat insulation sleeve The inlet is connected to a heat medium outlet provided on the first insulation sleeve. The apparatus for producing a metal compound by the ammonia method according to claim 8, wherein the top region of the decomposition precipitation tank is further provided with an observation hole. The apparatus for producing a metal compound by the ammonia method according to claim 8, wherein an inner diameter of a defoaming region of the decomposition precipitation tank is larger than an inner diameter of a top region. The apparatus for producing a metal compound by the ammonia method according to claim 8, wherein the top region, the defoaming region, and the rapid heating region of the decomposition and precipitation tank are cylindrical, and the upper and lower connection regions of the decomposition and precipitation tank It has a circular truncated cylinder shape, and the bottom region is a conical cylinder. The small diameter top surface of the upper connection region is connected to the bottom surface of the top region, and the small diameter top surface of the upper connection region is the same as the cross section of the top region. The large diameter bottom surface of the upper connection area is connected to the top surface of the defoaming area, and the large diameter bottom surface of the upper connection area is the same as the cross section of the defoaming area; the large diameter top surface of the lower connection area is connected to the The bottom surface of the defoaming region, the large diameter top surface of the lower connection region is the same as the cross-section of the defoaming region; the small diameter bottom surface of the lower connection region is connected to the top surface of the rapid heating region, and the lower connection The small diameter bottom surface of the zone is the same as the cross-section of the rapid heat zone; the top surface of the bottom zone is connected to the bottom surface of the quick heat zone, and the top surface of the bottom zone is the same as the cross-section of the rapid heat zone. The apparatus for producing a metal compound by the ammonia method according to claim 1, wherein the absorption device includes at least one absorption tower, and the absorption tower includes a connected top zone, an absorption zone, and a condensation zone from top to bottom; the top zone A mixed gas outlet is provided; a bottom of the absorption area is provided with a funnel-shaped bottom plate, and an edge of the funnel-shaped bottom plate is fixed to the inner wall of the absorption tower, and the outlet of the funnel-shaped bottom plate communicates with the condensation area; The absorption zone is provided with an air inlet corresponding to the funnel-shaped bottom plate; the absorption zone is provided with a first orifice plate and a second orifice plate, the first orifice plate is located above the intake hole, and the second hole A plate is located above the first orifice plate, and the edges of the first orifice plate and the second orifice plate are fixedly attached to the inner wall of the absorption tower; the absorption zone is provided with an absorption liquid inlet, and the absorption liquid inlet corresponds to It is located between the first orifice plate and the second orifice plate; absorbing materials are stacked on the first orifice plate and the second orifice plate; and the condensation zone is provided with a condensation device and an absorption liquid outlet. The device for producing a metal compound by the ammonia method according to claim 18, wherein the absorption device includes a plurality of absorption towers connected in series; a mixed gas outlet in a top region of the absorption tower is connected to an air inlet of another absorption tower. The device for producing a metal compound by the ammonia method according to claim 19, wherein the device for producing the metal compound by the ammonia method further includes an ammonium carbonate solution storage tank and a water supply device; and a reflux liquid inlet is also provided in the top region of the absorption tower. The absorption liquid outlet of the absorption tower is connected to the reflux liquid inlet of the previous absorption tower, the reflux liquid inlet of the first absorption tower is connected to the ammonium carbonate storage tank, and the reflux liquid inlet of the last absorption tower is connected to the water supply device. The apparatus for producing a metal compound by the ammonia method according to claim 20, wherein the ammonium carbonate solution storage tank is connected to the leaching tank. The device for producing a metal compound by the ammonia method according to claim 19, wherein a mixed gas outlet of the last absorption tower in the absorption device is connected to a pressure regulating device. The apparatus for producing a metal compound by the ammonia method according to claim 22, wherein the pressure regulator is a roots blower. The device for producing a metal compound by the ammonia method according to claim 19, wherein the absorption device includes four or more absorption columns connected in series. The apparatus for producing a metal compound by the ammonia method according to any one of claims 18 to 24, wherein an absorption liquid outlet of the absorption tower is connected to an absorption liquid inlet of the absorption tower through a pipeline provided with a lift pump. The device for producing a metal compound by the ammonia method according to claim 18, wherein an absorption liquid inlet of the absorption tower is connected to a spray pipe provided in the absorption tower, and the spray pipe is correspondingly located below the second orifice plate. . The device for producing a metal compound by the ammonia method according to claim 18, wherein the condensation device of the absorption device is a condensation coil group including a plurality of condensation coils connected in series. The device for producing a metal compound by the ammonia method according to claim 18, wherein the condensation zone of the absorption tower is provided with a cooling medium inlet and a cooling medium outlet, the cooling medium inlet is connected to the inlet of the condensation device, and the cooling medium outlet is connected to the Outlet of the condensing unit. A production process for an apparatus for producing a metal compound by an ammonia method according to any one of claims 1 to 28, comprising the steps of: leaching complexing reaction: adding a metal raw material to a metal feeding zone of the leaching tank, Then, ammonium carbonate solution is added to the leaching tank, and air is blown into the inside of the leaching tank through the reaction gas inlet and the circulation pipe. The blasted air is fully reacted with the ammonium carbonate solution in the circulation pipe, and the gas is released. After the reaction gas outlet of the leaching tank is condensed and enters the absorption device, the solution is pushed out of the circulation tube by the air to contact the metal raw material for the complexation reaction. At the same time, the solution also passes through the holes of the orifice plate and the circulation holes provided on the isolation sleeve. It flows into the bottom of the orifice plate, and then enters the circulation tube through the lower opening of the circulation tube to enter the circulation tube circulation reaction until the metal content reaches the standard; heating decomposition reaction: after filtering the metal ammonia complex solution obtained in the leaching tank, it is discharged from the decomposition sedimentation tank The feeding port is added to the decomposition sedimentation tank, heated by the heating coil group in the decomposition sedimentation tank, and air is blown in from the air stirring tube at the same time to decompose the sedimentation. The solution was stirred after the decomposition flows out from the decomposition of a metal compound precipitation tank discharge opening; Scrubber: precipitation vessel exploded decomposition gas generated by the reaction was cooled absorption into the absorbent means.