TWM550825U - Decomposition and sedimentation tank for producing metal compounds by ammonia method - Google Patents

Description

Ammonia process for the production of decomposition catalysts for metal compounds

This creation is about the field of chemical equipment, specifically the decomposition sedimentation tank for the production of metal compounds by the ammonia method.

At present, metal compounds including nickel carbonate, zinc carbonate, (active) copper oxide, and copper carbonate have long production processes, large energy consumption, complicated equipment structure, and various disadvantages in the production process. For example, active copper oxide has the characteristics of high purity, small particle size, large specific surface area, fast dissolution rate in the acid specified by the electroplating industry, and many specific energy and great potential application value in the fields of electronics and catalysis. Usually, the production of high-purity active copper oxide powder is mainly carried out by carbonate calcination. Due to the long production process of the calcined (calcining) method of carbonate, the subsequent washing is difficult, the purity of the product is not high, the dispersibility is not good, and the crystal is sintered. The product caused by grain coarsening is not high in activity, relatively high in cost, and has high-salt wastewater.

Regarding the production method of active copper oxide, the following two kinds are introduced in some patents disclosed at present: (1) Chinese Patent Application No. 01127175.2 "Processing Method for Producing Active Copper Oxide by Low Temperature Oxidation Wet Decomposition", the patent case is sulfuric acid Copper and copper materials are used as raw materials, and oxidized at a low temperature of 80 ° C to 85 ° C to obtain copper sulfate crystals, and then the solution is reacted with sodium hydroxide, and subjected to ball milling, pressure filtration, washing, drying, pulverization, etc. Active copper oxide is produced. (2) Chinese Patent Application No. 200710076208.1 "Method and Apparatus for Producing Copper Oxide/Copper Sulfate by Circuit Board Etching Liquid Recovery", which is a method for producing copper oxide by vaporizing ammonia from an alkaline etching waste liquid.

The above preparation methods all have the disadvantages of manufacturing, complicated equipment and high energy consumption, and a large amount of washing wastewater is generated, which brings a lot of troubles to the subsequent treatment.

In order to solve the above problems of production and manufacture, an environmentally friendly ammonia method for producing a metal compound is provided, and a decomposition method for producing a metal compound by an ammonia method suitable for the method is specifically provided.

The present invention provides a decomposition and sedimentation tank for producing a metal compound by an ammonia method, comprising: a sedimentation tank shell comprising a top zone connected to each other from top to bottom, an upper connection zone, a defoaming zone, a lower connection zone, a first hot zone and a 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 opening; the inner diameter of the defoaming zone is greater than the speed An inner diameter of the hot zone; an orifice plate provided with an opening, disposed in the sedimentation tank casing and located below the bottom of the rapid heating zone, the edge of the orifice plate being fitted and fixed to the inner wall of the sedimentation tank casing; An air agitating tube disposed inside the precipitation tank housing, one end of the air agitating tube is connected to the air inlet, and the other end is inserted through the opening of the orifice plate and extends into the bottom region below the orifice plate; A heating coil set is fixed to the orifice plate and located in the hot zone.

The decomposition precipitation tank for producing a metal compound by the aforementioned ammonia method further includes the following technical features: The heat medium inlet communicates with an inlet of the heating coil group, and the heat medium outlet communicates with an outlet of the heating coil group.

The heating coil set includes a plurality of heating coils in series.

The inner diameter of the defoaming zone is 1.1 times or more of the inner diameter of the hot zone.

The inner diameter of the defoaming zone is 1.1 to 5 times the inner diameter of the hot zone.

Further comprising a first thermal insulation sleeve sleeved on the outer side of the precipitation tank housing and at a position where the casing group should be heated, a heat medium inlet of the first thermal insulation sleeve is connected to the heat medium outlet of the rapid heating zone .

Further comprising a second thermal insulation sleeve sleeved on the outer side of the bottom region, a heat medium inlet of the second thermal insulation sleeve communicates with a heat medium outlet of the first thermal insulation sleeve.

The top area is provided with an observation hole.

The inner diameter of the defoaming zone is greater than the inner diameter of the top zone.

The top zone, the defoaming zone, and the hot zone are cylindrical, the upper connecting zone and the lower connecting zone are in the shape of a truncated cylinder, the bottom zone is a conical cylinder; the small diameter top surface of the upper connecting zone Connecting the bottom surface of the top region, 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 region is connected to the top surface of the defoaming region, and the large diameter bottom surface of the upper connection region The same as the cross section of the defoaming zone; the large diameter top surface of the lower connecting zone is connected to the bottom surface of the defoaming zone, the large diameter top surface of the lower connecting zone is the same as the cross section of the defoaming zone; a small diameter bottom surface is connected to the top surface of the rapid heating zone, the small diameter bottom surface of the lower connection zone is the same as the cross section of the rapid heating zone; the top surface of the bottom zone is connected to the bottom surface of the hot zone, and the top surface of the bottom zone With the speed zone The cross section is the same.

The creation can achieve the following technical effects: the air agitation function of the creation causes the generated metal compound to not precipitate, and the air that is blown in (the blower enters the gas) can take away a large amount of ammonia when it rises to the liquid surface. It reduces the resistance of ammonia volatilization in the liquid and reduces the possibility of ammonia being absorbed by the solution to form ammonia water. In addition, the position of the first heat insulating sleeve and the second heat insulating sleeve, and the heat medium that originally entered the heating coil group are used again to realize a heat utilization type.

1‧‧‧Sedimentation tank shell

10‧‧‧ top area

100‧‧‧ mixed gas outlet

101‧‧‧ observation hole

11‧‧‧Uplink area

110‧‧‧Air inlet

111‧‧‧Feeding port

12‧‧‧Defoaming zone

13‧‧‧Under connection area

14‧‧ ‧ fast hot zone

140‧‧‧Hot media inlet

141‧‧‧Hot media export

15‧‧‧ bottom area

150‧‧‧ discharge opening

2‧‧‧ Orifice

3‧‧‧Air mixing tube

4‧‧‧Heating coil set

40‧‧‧heating coil

5‧‧‧First Insulation Sleeve

50‧‧‧Hot media inlet

51‧‧‧Hot media outlet

6‧‧‧Second insulation casing

60‧‧‧Heat medium inlet

The first picture is a schematic diagram of the structure of the creation.

The second picture is a schematic diagram of the process of producing metal compounds in this creation.

As shown in the second figure, the principle of producing metal compounds (including copper oxide, copper carbonate, zinc carbonate and nickel carbonate) by ammonia method is as follows: metal (copper, nickel, zinc, etc.), ammonium carbonate solution (hydrogen carbonate) The mixed solution of the aqueous ammonium solution and the aqueous ammonia reacts with oxygen to form a metal complex, and the metal complex is heated to generate ammonia gas and metal oxide (or metal carbonate) depending on the heating temperature.

Taking the preparation of active copper oxide as an example, the following steps are included: (1) leaching complexation reaction: taking electrolytic copper, adding ammonium carbonate solution (mixed solution of ammonium hydrogencarbonate aqueous solution and ammonia water), and bubbling air (blower blown in) Air, the above description takes air as an example, or simply adopts oxygen), and performs a complexation reaction until the copper content in the reaction liquid reaches the standard to obtain a copper ammonium solution. The reaction equation is as _{follows: Cu + 2NH 4 HCO 3 +} 2NH 3 + O 2 = Cu (NH 3) 4 CO 3 + 2H 2 O. (2) The copper ammonia solution obtained in the step (1) is thermally decomposed to obtain copper carbonate or copper oxide (a copper carbonate is calcined (calcined) to obtain active copper oxide). (3) The exhaust gas is collected, and the gas generated by the above heating reaction is collected, and the gas referred to above is ammonia gas and is condensed to become ammonia water, and then collected.

The ammonia method provides a decomposition and precipitation tank for a metal compound, which is used in the above-mentioned preparation of a metal complex (copper ammonium solution) for use in a thermal decomposition reaction step.

As shown in the first figure, the decomposition process tank for producing a metal compound by the ammonia method comprises: a sedimentation tank housing 1, which comprises a top region 10 connected to each other from top to bottom, an upper connection region 11, and an elimination. a bubble region 12, a lower connection region 13, a first heat zone 14 and a bottom zone 15; the top zone 10, the defoaming zone 12, the speed zone 14 is cylindrical, and the upper connection zone 11 is connected to the bottom The zone 13 is in the shape of a truncated cone, and the bottom zone 15 has a conical cylindrical shape. The inner diameter of the defoaming zone 12 is larger than the inner diameter of the hot zone 14. The inner diameter of the defoaming zone 12 is 1.1 times or more of the inner diameter of the hot zone 14. The inner diameter of the defoaming zone 12 is The inner diameter of the hot zone 14 is 1.1 to 5 times (this arrangement can effectively achieve defoaming and gas-liquid separation). The inner diameter of the defoaming zone 12 is larger than the inner diameter of the top zone 10; the small diameter top surface of the upper connection zone 11 is connected to the bottom surface of the top zone 10, and the small diameter top surface of the upper connection zone 11 and the top zone 10 The cross-section is the same; the large-diameter bottom surface of the upper connecting portion 11 is connected to the top surface of the defoaming region 12, and the large-diameter bottom surface of the upper connecting portion 11 is the same as the cross-section of the defoaming region 12; The large diameter top surface is connected to the bottom surface of the defoaming zone 12, and the large diameter top surface of the lower connection zone 13 is the same as the cross section of the defoaming zone 12; the small diameter bottom surface of the lower connection zone 13 is connected to the top of the rapid heating zone 14. a small diameter bottom surface of the lower connection region 13 and the speed The hot zone 14 has the same cross section; the top surface of the bottom zone 15 is connected to the bottom surface of the hot zone 14, the top surface of which is the same as the cross section of the zone.

The top region 10 is provided with a mixed gas outlet 100 and an observation hole 101; the upper connecting portion 11 is provided with an air inlet 110 and a feeding port 111; and the bottom portion 15 is provided with a discharge opening 150.

An orifice plate 2 having an opening (the orifice plate 2 is a plate-like structure provided with a plurality of through holes) is disposed in the sedimentation tank housing 1 and located below the bottom of the rapid heating zone 14, the orifice plate 2 The edge is attached to the inner wall of the settling tank housing 1.

An air agitating tube 3 is disposed inside the precipitation tank housing 1. One end of the air agitating tube 3 is connected to the air inlet 110, and the other end passes through the opening of the orifice plate 2 and extends below the orifice plate 2. Inside the bottom zone 15.

And a heating coil assembly 4 comprising a plurality of heating coils 40 connected in series, which are fixed to the orifice plate 2 and located in the hot zone 14.

The hot zone 14 of the settling tank housing 1 is provided with a heat medium inlet 140 and a heat medium outlet 141. The heat medium inlet 140 communicates with an inlet (not shown) of the heating coil group 4, and the heat medium outlet 141 The outlet of the heating coil group 4 (not shown) is connected.

Further comprising a first thermal insulation sleeve 5, which is sleeved on the outer side of the precipitation tank housing 1 and the position where the casing group 4 should be heated, and a heat medium inlet 50 of the first thermal insulation sleeve 5 communicates with the rapid heat The heat medium outlet 141 of the zone 14 (not shown).

Further comprising a second thermal insulation sleeve 6 disposed outside the bottom region 15 , a heat medium inlet 60 of the second thermal insulation sleeve 6 communicating with the first thermal insulation sleeve 5 A heat medium outlet 51.

Taking the production of active copper oxide as an example, the decomposition and precipitation process in the decomposition and precipitation tank of the metal compound produced by the ammonia method is as follows: the filtered copper ammonia complex solution enters the decomposition sedimentation tank from the feed port 111, and the air is stirred by the air. 3 The incoming air is evenly distributed through the bottom plate 2 for bubbling agitation (injecting gas into the solution to generate bubbles and simultaneously tumbling the solution), and the copper ammonia complex solution is heated in the hot zone 14 by the coil unit 4 Rapid heating (the heat medium in the heating coil group 4 can be steam), when the solution reaches a certain temperature, it decomposes to form copper carbonate (or copper oxide) and mixed ammonia gas, and the copper carbonate (or copper oxide) is stirred under air. Suspended in solution. The large amount of foam generated by the rapid decomposition of ammonia gas is defoamed and gas-liquid separated in the defoaming zone 12, and the separated mixed ammonia gas is discharged through the mixed gas outlet 100 to the condenser to be condensed into mixed ammonia water.

The stirring function of the air agitating tube 3 of the decomposition tank of the present invention causes the generated metal compound (copper carbonate) not to precipitate, and the air that is blown in takes up a large amount of ammonia gas when rising, and reduces the resistance of the ammonia vapor in the liquid. Reduce the possibility of ammonia being secondarily absorbed by the solution to form ammonia. At the same time, the set positions of the first heat insulating sleeve 5 and the second heat insulating sleeve 6 and the heat medium which originally entered the heating coil group 4 are used again to realize a heat utilization type.

1‧‧‧Sedimentation tank shell

10‧‧‧ top area

100‧‧‧ mixed gas outlet

101‧‧‧ observation hole

11‧‧‧Uplink area

110‧‧‧Air inlet

111‧‧‧Feeding port

12‧‧‧Defoaming zone

13‧‧‧Under connection area

14‧‧ ‧ fast hot zone

140‧‧‧Hot media inlet

141‧‧‧Hot media export

15‧‧‧ bottom area

150‧‧‧ discharge opening

2‧‧‧ Orifice

3‧‧‧Air mixing tube

4‧‧‧Heating coil set

40‧‧‧heating coil

5‧‧‧First Insulation Sleeve

50‧‧‧Hot media inlet

51‧‧‧Hot media outlet

6‧‧‧Second insulation casing

60‧‧‧Heat medium inlet

Claims (10)

The invention discloses a decomposition and sedimentation tank for producing a metal compound by an ammonia method, comprising: a sedimentation tank shell comprising a top region connected to each other from top to bottom, an upper connecting region, a defoaming region, a lower connecting region and a first hot zone. And a 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 opening; the inner diameter of the defoaming zone is larger than the inner zone of the rapid heating zone a hole plate having an opening, which is disposed in the sedimentation tank housing and located below the bottom of the rapid heating zone, the edge of the orifice plate being fitted and fixed to the inner wall of the sedimentation tank housing; an air mixing tube Provided in the interior of the precipitation tank, one end of the air agitating tube is connected to the air inlet, and the other end passes through the opening of the orifice plate and extends into the bottom region below the orifice plate; and a heating coil A set, which is fixed to the orifice plate and located in the hot zone. The ammonia method for producing a metal compound decomposition sedimentation tank according to claim 1, wherein the rapid heating zone of the precipitation tank casing is provided with a heat medium inlet and a heat medium outlet, and the heat medium inlet communicates with the inlet of the heating coil group. The heat medium outlet communicates with the outlet of the heating coil group. The decomposition process tank for producing a metal compound according to the ammonia method of claim 1 or claim 2, wherein the heating coil group comprises a plurality of heating coils connected in series. The decomposition method of the metal compound according to claim 1 or claim 2, wherein the inner diameter of the defoaming zone is 1.1 times or more of the inner diameter of the hot zone. The ammonia method according to claim 4, wherein the inner diameter of the defoaming zone is 1.1 to 5 times the inner diameter of the hot zone. The decomposition process tank for producing a metal compound by the ammonia method according to claim 1 or claim 2, further comprising a first heat insulating sleeve which is sleeved in the precipitation tank shell and The outside of the position of the casing set should be heated, a heat medium inlet of the first insulated casing communicating with the heat medium outlet of the hot zone. The decomposition process tank for producing a metal compound by the ammonia method according to claim 6, further comprising a second heat insulating sleeve disposed outside the bottom region, wherein a heat medium inlet of the second heat insulating sleeve communicates with the first A heat medium outlet of the thermal insulation sleeve. The ammonia method according to claim 1 produces a decomposition sedimentation tank of a metal compound, wherein the top zone is provided with an observation hole. The ammonia process as claimed in claim 1 is characterized in that the decomposition tank of the metal compound is produced, wherein the inner diameter of the defoaming zone is larger than the inner diameter of the top zone. The decomposition method of the metal compound according to claim 1 or claim 9, wherein the top zone, the defoaming zone, and the hot zone are cylindrical, and the upper connection zone and the lower connection zone are a round table cylindrical shape, the bottom portion is a conical cylindrical shape; a small diameter top surface of the upper connecting portion is connected to a bottom surface of the top portion, and a small diameter top surface of the upper connecting portion is the same as a cross section of the top portion; the upper connection a large diameter bottom surface of the zone is connected to the top surface of the defoaming zone, the large diameter bottom surface of the upper connection zone is the same as the cross section of the defoaming zone; the large diameter top surface of the lower connection zone is connected to the bottom surface of the defoaming zone, the lower The large diameter top surface of the connection zone is the same as the cross section of the defoaming zone; the small diameter bottom surface of the lower connection zone is connected to the top surface of the rapid heating zone, and the small diameter bottom surface of the lower connection zone and the cross section of the rapid heating zone The top surface of the bottom region is connected to the bottom surface of the hot zone, and the top surface of the bottom region is the same as the cross section of the hot zone.