CN115852172A - System and method for decomposing tantalum-niobium slurry - Google Patents
System and method for decomposing tantalum-niobium slurry Download PDFInfo
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Abstract
The invention provides a system and a method for decomposing tantalum-niobium slurry, wherein the system comprises: the device comprises a decomposition tank, a temperature transmitter, a pressure transmitter and a liquid level meter, wherein the decomposition tank is communicated with a slurry pipeline, an acid pipeline, a process water pipeline and a tail gas pipeline; and the PLC is in signal connection with the temperature transmitter, the pressure transmitter and the liquid level meter respectively, and is in signal connection with the acid metering pump and the process water pump respectively. The system and the method for decomposing the tantalum-niobium slurry can automatically pre-judge and automatically respond to the danger of accidents such as pot explosion and the like in the process of decomposing the tantalum-niobium slurry in time, and ensure the safe operation of the process of decomposing the tantalum-niobium slurry.
Description
Technical Field
The invention relates to the technical field of metal metallurgy, in particular to a system and a method for decomposing tantalum-niobium slurry.
Background
Tantalum and niobium belong to rare metals with high boiling point and high melting point, have the excellent characteristics of high strength, fatigue resistance, deformation resistance, corrosion resistance, easy heat conduction, superconductivity, unipolar conductivity, gas absorption and the like, and are widely applied to the industries of electronics, aerospace, machinery industry, atomic reactor and the like.
The main industrial minerals of tantalum and niobium are two types, one is tantalate and niobate, and the main mineral is tantalite; the other is titanium tantalate niobate, and the main minerals are pyrochlore, aplite and the like. The ore concentrate of tantalum and niobium is difficult to decompose by other acids except hydrofluoric acid, when the ore concentrate of tantalum and niobium is decomposed by hydrofluoric acid, the tantalum, niobium, titanium, silicon and iron in the ore concentrate enter the solution in the form of soluble components, and the rare earth and radioactive elements uranium and thorium remain in the slag, so that the rare earth, particularly uranium and thorium, which are main impurities in the ore can be separated from the tantalum and niobium at the initial stage of ore concentrate decomposition. And because sulfuric acid can react with partial impurities in the tantalum-niobium concentrate, and the volatilization loss of hydrofluoric acid in the decomposition process can be reduced, the tantalum-niobium smelter in China usually adopts hydrofluoric acid-sulfuric acid to decompose ores.
In the prior art, the research on the hydrofluoric acid-sulfuric acid decomposition of ores is mostly the research on parameters such as acid concentration, decomposition temperature, stirring rate and the like, and the research on the process of extracting tantalum and niobium is lacked, particularly the research on the analysis and the countermeasures of accidents such as pot explosion and the like in the process of extracting tantalum and niobium is lacked. Therefore, the system and the method for decomposing the tantalum-niobium slurry have important significance in providing the system and the method which are efficient and automatic control, can eliminate danger in time and ensure safe production.
Disclosure of Invention
Based on the above purpose, the present invention provides a system and a method for decomposing tantalum-niobium slurry, so as to solve or partially solve the above technical problems:
a tantalum-niobium slurry decomposition system comprising:
the system comprises a decomposition tank, a pipeline and a pipeline, wherein the decomposition tank is communicated with a slurry pipeline, an acid pipeline, a process water pipeline and a tail gas pipeline, the decomposition tank is provided with a temperature transmitter, a pressure transmitter and a liquid level meter, the acid pipeline is provided with an acid metering pump, and the process water pipeline is provided with a process water pump;
and the PLC is in signal connection with the temperature transmitter, the pressure transmitter and the liquid level meter respectively, and the PLC is in signal connection with the acid metering pump and the process water pump respectively.
Further, a slurry pump is arranged on the slurry pipeline and is in signal connection with the liquid level meter; and a breather valve is arranged on the tail gas pipeline.
Furthermore, the acid pipeline comprises a hydrofluoric acid pipeline and a concentrated sulfuric acid pipeline, a hydrofluoric acid metering pump is arranged on the hydrofluoric acid pipeline, and a concentrated sulfuric acid metering pump is arranged on the concentrated sulfuric acid pipeline.
Further, a stirrer is also arranged in the decomposition tank.
Based on the same inventive concept, the invention also provides a method for decomposing the tantalum-niobium slurry, which comprises the following steps:
after the bottoming process water is conveyed to the decomposing tank, starting a stirrer in the decomposing tank;
after the tantalum-niobium slurry is conveyed to the decomposition tank, conveying acid liquor into the decomposition tank at a preset acid liquor conveying speed, and carrying out acidolysis reaction on the tantalum-niobium slurry and the acid liquor to obtain acidolysis solution containing tantalum-niobium;
analyzing acidolysis reaction characteristics, and determining process parameters representing acidolysis reaction dangerousness, wherein the process parameters comprise temperature, pressure and liquid level change rate;
based on the process parameters, hazardous abatement operations are performed.
Further, after the tantalum-niobium slurry is conveyed to the decomposition tank, conveying the acid solution to the decomposition tank at a preset acid solution conveying speed, which specifically comprises the following steps:
starting a slurry pump to convey the tantalum-niobium slurry, and stopping the slurry pump when the liquid level of the decomposition tank reaches a slurry stop preset level value to finish the conveyance of the tantalum-niobium slurry;
and (3) after the tantalum-niobium slurry is conveyed for 2min to 5min, starting an acid metering pump, conveying the acid liquid into the decomposition tank at a preset acid liquid conveying speed, performing cumulative metering on the conveying amount of the acid liquid by using the acid metering pump, and stopping the acid metering pump when the cumulative metered conveying amount of the acid liquid reaches the preset acid liquid conveying amount value to finish conveying the acid liquid.
Further, the acid solution comprises hydrofluoric acid and concentrated sulfuric acid.
Further, based on the process parameters, the operation of eliminating the danger is carried out, which specifically comprises:
setting preset values for each parameter of temperature, pressure and liquid level change rate;
and when the real-time value of any one parameter of the temperature, the pressure and the liquid level change rate reaches the preset value of the process parameter, carrying out danger elimination operation, wherein the danger elimination operation comprises one or more of reducing the acid liquor conveying rate, stopping acid liquor conveying, conveying danger elimination process water and stopping danger elimination process water conveying.
Further, setting three preset values for each parameter of temperature, pressure and liquid level change rate, wherein the three preset values are respectively a speed reduction preset value, an acid stopping preset value and an acid stopping and water adding preset value, and the speed reduction preset value, the acid stopping preset value and the acid stopping and water adding preset value are sequentially increased;
when the real-time value of any one parameter of the temperature, the pressure and the liquid level change rate reaches the deceleration preset value of the process parameter, the acid liquor conveying rate is reduced;
when the real-time value of any one parameter of the temperature, the pressure and the liquid level change rate reaches the acid stopping preset value of the process parameter, stopping acid liquor conveying;
when the real-time value of any parameter of the temperature, the pressure and the liquid level change rate reaches the acid-stopping and water-adding preset value of the process parameter, the acid liquor conveying is stopped and the dangerous process water is conveyed.
From the above, the system and the method for decomposing the tantalum-niobium slurry provided by the invention have the following beneficial effects:
the process parameters for characterizing the risk of acidolysis reactions are proposed: temperature, pressure, and rate of change of liquid level. And arranging a PLC (programmable logic controller), wherein the PLC is in signal connection with the liquid level meter, the temperature transmitter and the pressure transmitter respectively to monitor the temperature, the pressure and the real-time value of the liquid level change rate, and the real-time value is compared with a preset value, and one or more operations of reducing the acid liquor conveying rate, stopping the acid liquor conveying, conveying danger-eliminating process water and stopping the danger-eliminating process water conveying are carried out according to the comparison result, so that the PLC is used for preventing accidents such as pot burst, explosion and the like in the acidolysis reaction process and ensuring the safe operation of the tantalum-niobium slurry decomposition process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a decomposition system of tantalum-niobium slurry according to an embodiment of the present invention.
In the figure: 1-a decomposition tank; 11-a temperature transmitter; 12-a pressure transmitter; 13-a liquid level meter; 14-a stirrer; 2-slurry pipeline; 21-slurry pump; 22-slurry shut-off valve; 3-process water pipeline; 31-a process water pump; 32-process water shut-off valve; 4-tail gas pipeline; 41-a breather valve; 5-a PLC controller; 6-hydrofluoric acid pipeline; 61-hydrofluoric acid metering pump; 7-concentrated sulfuric acid pipeline; 71-concentrated sulfuric acid metering pump.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings.
It should be noted that technical terms or scientific terms used in the embodiments of the present invention should have the ordinary meanings as understood by those having ordinary skill in the art to which the present invention belongs, unless otherwise defined. As used herein, the terms "first," "first," and the like, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items. "communication" or "communicating" and like terms are not limited to physical or mechanical communication, but may include electrical communication, whether direct or indirect. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
In the metallurgical industry of tantalum and niobium, the ore is decomposed by adopting hydrofluoric acid-sulfuric acid, the decomposition reaction is severe, and the hydrofluoric acid and concentrated sulfuric acid belong to strong corrosive acids, so that the possibility of accidents such as pot explosion and explosion is high, and the harm is huge. In the prior art, the occurrence of accidents such as boiling off a boiler, explosion and the like is expected to be reduced as much as possible by strictly controlling process parameters and improving the level of fine operation, such as accurately controlling the acid concentration, the acid amount, the reaction time and the like, and slowly adding a small amount of raw materials for many times, but the operations are only prevention and have limited effect, and a direct, effective and systematic accident risk prediction scheme and a coping means are not provided.
In view of this, one or more embodiments of the present invention provide a system and a method for decomposing a tantalum-niobium slurry, where the system and the method can automatically pre-determine and automatically respond to the danger of accidents such as pot explosion and explosion in the process of decomposing the tantalum-niobium slurry in time, so as to ensure the safe operation of the process of decomposing the tantalum-niobium slurry.
The technical solutions of one or more embodiments of the present invention will be described in detail below with reference to specific embodiments.
A tantalum-niobium slurry decomposition system comprising: a decomposition tank 1 and a PLC 5. Wherein, the decomposition tank 1 is a place for carrying out acidolysis reaction on the tantalum-niobium slurry and the acid liquor. The decomposing tank 1 is communicated with a slurry pipeline 2, an acid pipeline, a process water pipeline 3 and a tail gas pipeline 4. The slurry pipeline 2, the acid pipeline and the process water pipeline 3 are input channels of tantalum-niobium slurry, acid liquor and process water respectively. The tail gas line 4 is a gas inlet and outlet passage for maintaining a stable operating pressure in the decomposition tank 1. Be provided with temperature transmitter 11, pressure transmitter 12 and level gauge 13 on the decomposer 1, temperature transmitter 11 is arranged in the temperature of real-time display decomposer 1 liquid phase, and pressure transmitter 12 is arranged in the real-time pressure of showing gaseous phase in decomposer 1, and level gauge 13 is arranged in the real-time liquid level of showing in decomposer 1. An acid metering pump is arranged on the acid pipeline and used for metering acid liquor conveying amount, adjusting acid liquor conveying speed and starting and stopping acid liquor conveying, a process water pump 31 is arranged on the process water pipeline 3, and the process water pump 31 is used for starting and stopping process water conveying.
And the PLC 5 is respectively in signal connection with the temperature transmitter 11, the pressure transmitter 12 and the liquid level meter 13 so as to obtain the temperature, the pressure and the liquid level in the decomposition tank 1 in real time and directly compare the temperature and the pressure with preset values thereof. It is noted that the liquid level there is not directly compared to a preset level value, but the liquid level is converted into a liquid level change rate, where the liquid level change rate = liquid level change amount/time change amount, which is compared to a liquid level change rate preset value. The PLC 5 is respectively in signal connection with the acid metering pump and the process water pump 31, and one or more operations of reducing the acid liquor conveying speed, stopping acid liquor conveying, conveying danger-eliminating process water and stopping danger-eliminating process water conveying are carried out according to the comparison result of the real-time values of the temperature, the pressure and the liquid level change speed and the preset values, so that potential dangers such as pot explosion and explosion are eliminated.
In some embodiments, a slurry pump 21 is disposed on the slurry pipeline 2, and the slurry pump 21 is connected with the liquid level meter 13 in a signal linkage manner to automatically quantitatively input the tantalum-niobium slurry. The tail gas pipeline 4 is provided with a breather valve 41, and the constant operation pressure in the decomposition tank 1 is automatically maintained through the expiration and inspiration of the breather valve 41, namely, when the pressure in the decomposition tank 1 is too high, the pressure is timely released, and the decomposition tank 1 with too high pressure is prevented from bursting; when the pressure in the decomposition tank 1 is too small, gas is sucked in to ensure a constant operating pressure in the decomposition tank 1.
In some embodiments, in the tantalum-niobium decomposition process, the tantalum-niobium slurry is decomposed by using two acids, i.e., hydrofluoric acid and concentrated sulfuric acid. Therefore, the acid pipeline comprises a hydrofluoric acid pipeline 6 and a concentrated sulfuric acid pipeline 7, the hydrofluoric acid pipeline 6 is provided with a hydrofluoric acid metering pump 61, and the concentrated sulfuric acid pipeline 7 is provided with a concentrated sulfuric acid metering pump 71. The hydrofluoric acid pipeline 6 and the concentrated sulfuric acid pipeline 7 are respectively input channels of hydrofluoric acid and concentrated sulfuric acid, the hydrofluoric acid metering pump 61 is used for metering delivery capacity of the hydrofluoric acid, adjusting delivery rate of the hydrofluoric acid and starting and stopping delivery of the hydrofluoric acid, and the concentrated sulfuric acid metering pump 71 is used for metering delivery capacity of the concentrated sulfuric acid, adjusting delivery rate of the concentrated sulfuric acid and starting and stopping delivery of the concentrated sulfuric acid.
In some embodiments, an agitator 14 is further disposed in the decomposition tank 1 for stirring the tantalum-niobium slurry and the acid solution.
Based on the same inventive concept, the invention also provides a method for decomposing the tantalum-niobium slurry, which comprises the following steps:
step 101: after the bottoming process water is delivered to the decomposition tank 1, the stirrer 14 in the decomposition tank 1 is started.
In this step, the bottoming process water is fed from the process water line 3 into the decomposer 1. A small amount of process water is conveyed to bottom so as to wet the wall surface of the decomposition tank 1, so that the direct input of the tantalum-niobium slurry is prevented, the tantalum-niobium slurry is prevented from being bonded with the wall surface, the wetting is uneven, and the slurry is wasted.
Step 102: and (3) after the tantalum-niobium slurry is conveyed to the decomposition tank 1, conveying acid liquor to the decomposition tank 1 at a preset acid liquor conveying speed, and carrying out acidolysis reaction on the tantalum-niobium slurry and the acid liquor to obtain acidolysis solution containing tantalum and niobium.
In this step, after the stirrer 14 is started, the tantalum-niobium slurry is added, and if the stirrer 14 is started after the tantalum-niobium slurry is added, the tantalum-niobium slurry is large in amount and viscous, so that the stirring is not uniform, and the stirrer motor may be burnt due to large starting resistance of the stirrer 14. After the tantalum-niobium slurry is added, acid liquor is added, if the acid liquor is added firstly, the acid liquor amount is large, and the tantalum-niobium slurry amount is small, the reaction is violent, the heat release amount is large, and the acid liquor can splash to cause danger.
Step 102, specifically comprising:
step 1021: and (3) adding the bottoming process water to a preset liquid level of the bottoming process water, starting the slurry pump 21 to convey the tantalum-niobium slurry, and stopping the slurry pump 21 when the liquid level of the decomposition tank 1 reaches a slurry stop preset liquid level value to finish the conveyance of the tantalum-niobium slurry. The liquid level meter 11 in the decomposing tank 1 is connected with the slurry pump 21 through electric signals to form a linkage relation, the input quantity of the tantalum-niobium slurry is controlled through the slurry stopping preset liquid level value, and the quantitative automatic shutdown input of the tantalum-niobium slurry is realized.
Step 1022: and (3) after the tantalum-niobium slurry is conveyed for 2min to 5min, starting an acid metering pump, conveying the acid liquid into the decomposition tank 1 at a preset acid liquid conveying speed, carrying out cumulative metering on the conveying capacity of the acid liquid by the acid metering pump, and stopping the acid metering pump when the cumulative metered conveying capacity of the acid liquid reaches the preset acid liquid conveying capacity value to finish conveying the acid liquid. The acid liquor is conveyed by a metering pump with metering and flow regulating functions, because the consumption of hydrofluoric acid and concentrated sulfuric acid required by each ton of concentrate acidolysis is relatively less for the tantalum-niobium slurry decomposition process1230 to 1300L hydrofluoric acid/per ton concentrate and 480 to 520L concentrated sulfuric acid/per ton concentrate, the consumption of the hydrofluoric acid and the concentrated sulfuric acid is usually less than 2.0m 3 And the metering pump is used for greatly saving the cost compared with a metering pump which is provided with a combination of a centrifugal pump, a flowmeter and a regulating valve. In addition, because hydrofluoric acid and concentrated sulfuric acid are strong corrosive acid, the selection material difficulty of flowmeter, governing valve, and in the actual production process, tantalum niobium enterprise can pass through the plastic cylinder usually, and manual control hydrofluoric acid and concentrated sulfuric acid delivery rate and delivery capacity, the measurement is inaccurate, and greatly reduced production efficiency.
In some embodiments, the acid solution comprises hydrofluoric acid and concentrated sulfuric acid. More specifically, after the tantalum-niobium slurry is conveyed for 2min to 5min, the hydrofluoric acid metering pump 61 is started, hydrofluoric acid is conveyed into the decomposition tank 1 at a preset hydrofluoric acid conveying rate, the hydrofluoric acid metering pump 61 performs cumulative metering on the conveying amount of the hydrofluoric acid, and when the conveying amount of the cumulatively metered hydrofluoric acid reaches the preset hydrofluoric acid conveying amount value, the hydrofluoric acid metering pump 61 is closed, so that quantitative and constant-speed conveying of the hydrofluoric acid is completed. And then starting the concentrated sulfuric acid metering pump 71, delivering the concentrated sulfuric acid into the decomposition tank 1 at a preset concentrated sulfuric acid delivery rate, performing accumulated metering on the delivery capacity of the concentrated sulfuric acid by the concentrated sulfuric acid metering pump 71, and stopping the concentrated sulfuric acid metering pump 71 when the delivery capacity of the accumulated metered concentrated sulfuric acid reaches a preset concentrated sulfuric acid delivery capacity value, so as to finish quantitative and constant-speed delivery of the concentrated sulfuric acid. That is, hydrofluoric acid is first conveyed, and concentrated sulfuric acid is then conveyed.
Step 103: and analyzing the acidolysis reaction characteristics, and determining process parameters representing the acidolysis reaction risk, wherein the process parameters comprise temperature, pressure and liquid level change rate.
The acidolysis reaction is a series of violent decomposition or oxidation reactions, compounds of elements such as Ta (tantalum), nb (niobium), ti, fe, ca, mg, al and the like in the materials are decomposed and oxidized into substances such as sulfate and the like by hydrofluoric acid or concentrated sulfuric acid, and the chemical reaction comprises the following steps: ta 2 O 5 +14HF=2H 2 TaF 2 +5H 2 O，Nb 2 O 5 +14HF=2H 2 NbF 2 +5H 2 O,SiO 2 +6HF=H 2 SiF 6 +2H 2 O,TiO 2 +6HF=H 2 TiF 6 +2H 2 O,CaO+H 2 SO 4 =CaSO 4 ↓+5H 2 O,R 2 O 3（ Rare earth element ） +6HF=2RF 3 ↓+3H 2 O，FeO+H 2 SO 4 =FeSO 4 +5H 2 O, and the like. In the process of decomposing the tantalum-niobium slurry, oxidation heat release, acid liquor dilution heat, gas sensible heat and the like are accompanied, part of the heat except for heating materials is discharged through discharged air, water vapor and a small amount of acid mist, theoretically, the inlet and the outlet of the system are balanced, and the temperature and the pressure are stable.
However, in the acidolysis reaction process, due to various uncontrollable and difficult-to-control reasons such as uneven stirring, material feeding rate, material feeding amount change, feeding component change and the like, multiple segmental chemical reactions may occur in the reaction, and once the multiple segmental chemical reactions occur, the first-stage reaction materials are quickly gathered at the upper part due to the action of the porous layer and the airflow to form a covering layer, the airflow of the later-stage reaction materials is blocked by the resistance of the covering layer, the temperature and the pressure of the material liquid are increased, the boiling point is further increased, the heat energy and the static pressure are rapidly increased, the material liquid is heated and vaporized, and the gas phase pressure is rapidly increased. In addition, air, water vapor and acid mist carry solid particles when discharged, and the gas in the system is slowly discharged or even cannot be discharged because the discharge channel is gradually blocked after long-term accumulation, so that the gas phase pressure is increased sharply. Once the temperature and the pressure reach the final critical values, the decomposition tank 1 deforms, cracks and explodes, the materials are sprayed out, and hydrofluoric acid and concentrated sulfuric acid leak to cause personnel injury and serious production safety accidents.
Thus, the process parameters characterizing the risk of acidolysis reaction are determined: temperature, pressure. In addition, the liquid phase boils when the temperature rises, and bubbles are accumulated on the surface of the liquid and rise in a stacking way, so that the determined process parameters for representing the acidolysis reaction risk also comprise the liquid level change rate, and the liquid level change rate reflects the speed of the liquid level change.
Step 104: based on the process parameters, hazardous abatement operations are performed. The method specifically comprises the following steps:
step 1041, setting preset values for each parameter of temperature, pressure, and liquid level change rate;
1042, when the real-time value of any one of the temperature, the pressure and the liquid level change rate reaches the preset value of the process parameter, carrying out danger elimination operation, wherein the danger elimination operation comprises one or more of reducing the acid liquor conveying rate, stopping acid liquor conveying, conveying danger elimination process water and stopping danger elimination process water conveying, and the danger elimination process water is input into the decomposition tank 1 from the process water pipeline 3. In normal operation, the decomposition tank 1 is kept at the normal operating values of the temperature, pressure and liquid level change rate, once the real-time values of the temperature, pressure and liquid level change rate are higher than the normal operating values of the temperature, pressure and liquid level change rate, accidents such as pot burst and explosion will occur, and the higher the value of the height is, the higher the danger is, and different countermeasures for eliminating the danger are taken. Therefore, the preset values of the process parameters at different levels are set, and one or more different countermeasures of reducing the acid liquor conveying speed, stopping acid liquor conveying, conveying danger-eliminating process water and stopping danger-eliminating process water conveying are adopted according to the preset values at different levels.
More specifically, three preset values are set for each parameter of temperature, pressure and liquid level change rate, namely, a speed reduction preset value, an acid stop preset value and an acid stop and water addition preset value are respectively set, and the speed reduction preset value, the acid stop preset value and the acid stop and water addition preset value are sequentially increased, namely, differences among the speed reduction preset value, the acid stop and water addition preset value and a parameter normal-condition operating value are sequentially increased, for example, the normal-condition operating value of the temperature is 40-50 ℃, the speed reduction preset value is 70 ℃, the acid stop preset value is 80 ℃ and the acid stop and water addition preset value is 90 ℃.
And when the real-time value of any one parameter of the temperature, the pressure and the liquid level change rate reaches the deceleration preset value of the process parameter, reducing the acid liquor conveying rate until the real-time value of the process parameter reaches the normal-condition operation value during normal operation, and restoring the acid liquor conveying rate to the previous preset acid liquor conveying rate.
And when the real-time value of any parameter of the temperature, the pressure and the liquid level change rate reaches the acid stop preset value of the process parameter, stopping acid liquor conveying until the real-time value of the process parameter reaches the normal-condition operation value during normal operation, and conveying the acid liquor at the previous preset acid liquor conveying rate again.
And when the real-time value of any parameter of the temperature, the pressure and the liquid level change rate reaches the preset acid adding and water stopping value of the process parameter, stopping acid liquor conveying and conveying dangerous process water until the real-time value of the process parameter reaches the normal operating value in normal operation, stopping input of the dangerous process water, and conveying the acid liquor at the previous preset acid liquor conveying rate again.
In addition, if any operation of reducing the acid liquor conveying speed, stopping the acid liquor conveying and conveying the hazardous process water is performed, and the pressure is not reduced to the normal operating value during the normal operation, the tail gas pipeline 4 may be seriously blocked by large-particle impurities, and at the moment, all the feeding and discharging operations which are performed are stopped, including stopping the hazardous process water conveying, and the production is performed after the tail gas pipeline 4 is cleaned.
Example 1
Step 1: the process water pump 31 is started, and after the bottoming process water is delivered to the decomposition tank 1, the stirrer 14 in the decomposition tank 1 is started.
Step 2: and starting the slurry pump 21 to convey the tantalum-niobium slurry, and stopping the slurry pump 21 when the liquid level of the decomposition tank 1 reaches a slurry stop preset level value to finish conveying the tantalum-niobium slurry.
And 3, step 3: and (3) after the tantalum-niobium slurry is conveyed for 2min to 5min, starting a hydrofluoric acid metering pump 61, conveying hydrofluoric acid into the decomposition tank 1 at a preset hydrofluoric acid conveying speed, carrying out accumulative metering on the conveying capacity of the hydrofluoric acid by the hydrofluoric acid metering pump 61, and stopping the hydrofluoric acid metering pump 61 when the conveying capacity of the hydrofluoric acid reaches a hydrofluoric acid conveying capacity preset value, so as to finish quantitative and constant-speed conveying of the hydrofluoric acid.
And 4, step 4: and then starting the concentrated sulfuric acid metering pump 71, delivering the concentrated sulfuric acid into the decomposition tank 1 at a preset concentrated sulfuric acid delivery rate, performing accumulated metering on the delivery capacity of the concentrated sulfuric acid by the concentrated sulfuric acid metering pump 71, and stopping the concentrated sulfuric acid metering pump 71 when the delivery capacity of the accumulated metered concentrated sulfuric acid reaches a preset concentrated sulfuric acid delivery capacity value, so as to finish quantitative and constant-speed delivery of the concentrated sulfuric acid.
And 5: three preset values are set for each parameter of temperature, pressure and liquid level change rate, wherein the three preset values are respectively a speed reduction preset value, an acid stopping preset value and an acid stopping and water adding preset value. The temperature reduction preset value is 70 ℃, the acid stop preset value is 80 ℃, and the acid stop water addition preset value is 90 ℃; the pressure reduction preset value is 50KPa, the acid stopping preset value is 100KPa, and the acid stopping and water adding preset value is 110KPa; the speed reduction preset value of the liquid level change rate is 100mm/h, the acid stopping preset value is 200mm/h, and the acid stopping and water adding preset value is 300mm/h.
Step 6: when hydrofluoric acid or concentrated sulfuric acid is conveyed, when the real-time value of any parameter of temperature, pressure and liquid level change rate reaches 70 ℃, or 50KPa, or 100mm/h, the acid liquor conveying rate is reduced; when the real-time value of any parameter of the temperature, the pressure and the liquid level change rate reaches 80 ℃, or 100KPa, or 200mm/h, stopping acid liquor conveying; when the real-time value of any parameter of the temperature, the pressure and the liquid level change rate reaches 90 ℃, or 110KPa, or 300mm/h, the acid liquor transportation is stopped and the dangerous process water is added.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, is limited to these examples; within the idea of the invention, also technical features in the above embodiments or in different embodiments may be combined, steps may be implemented in any order, and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The embodiments of the invention are intended to embrace all such alternatives, modifications and variances that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalents, improvements, and the like that may be made without departing from the spirit or scope of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A tantalum-niobium slurry decomposition system, comprising:
the system comprises a decomposition tank, a pipeline and a pipeline, wherein the decomposition tank is communicated with a slurry pipeline, an acid pipeline, a process water pipeline and a tail gas pipeline, the decomposition tank is provided with a temperature transmitter, a pressure transmitter and a liquid level meter, the acid pipeline is provided with an acid metering pump, and the process water pipeline is provided with a process water pump;
and the PLC is in signal connection with the temperature transmitter, the pressure transmitter and the liquid level meter respectively, and the PLC is in signal connection with the acid metering pump and the process water pump respectively.
2. The system of claim 1, wherein the tantalum-niobium slurry decomposition system,
a slurry pump is arranged on the slurry pipeline and is in signal connection with the liquid level meter;
and a breather valve is arranged on the tail gas pipeline.
3. The system of claim 1, wherein the tantalum-niobium slurry decomposition system,
the acid pipeline comprises a hydrofluoric acid pipeline and a concentrated sulfuric acid pipeline, a hydrofluoric acid metering pump is arranged on the hydrofluoric acid pipeline, and a concentrated sulfuric acid metering pump is arranged on the concentrated sulfuric acid pipeline.
4. The system of claim 1, wherein an agitator is further disposed in the decomposition tank.
5. A method for decomposing a tantalum-niobium slurry based on the system for decomposing a tantalum-niobium slurry of any one of claims 1 to 4, comprising the steps of:
after the bottoming process water is conveyed to the decomposing tank, starting a stirrer in the decomposing tank;
after the tantalum-niobium slurry is conveyed to the decomposition tank, conveying acid liquor to the decomposition tank at a preset acid liquor conveying speed, and carrying out acidolysis reaction on the tantalum-niobium slurry and the acid liquor to obtain acidolysis solution containing tantalum-niobium;
analyzing acidolysis reaction characteristics, and determining technological parameters representing acidolysis reaction dangerousness, wherein the technological parameters comprise temperature, pressure and liquid level change rate;
based on the process parameters, hazardous abatement operations are performed.
6. The method for decomposing tantalum-niobium slurry as claimed in claim 5, wherein after the tantalum-niobium slurry is delivered to the decomposition tank, the acid solution is delivered to the decomposition tank at a predetermined acid solution delivery rate, and the method comprises the following steps:
starting a slurry pump to convey the tantalum-niobium slurry, and stopping the slurry pump when the liquid level of the decomposition tank reaches a slurry stop preset level value to finish the conveyance of the tantalum-niobium slurry;
and (3) after the tantalum-niobium slurry is conveyed for 2min to 5min, starting an acid metering pump, conveying the acid liquid into the decomposition tank at a preset acid liquid conveying speed, performing cumulative metering on the conveying amount of the acid liquid by using the acid metering pump, and stopping the acid metering pump when the cumulative metered conveying amount of the acid liquid reaches the preset acid liquid conveying amount value to finish conveying the acid liquid.
7. The method of claim 6, wherein the acid solution comprises hydrofluoric acid and concentrated sulfuric acid.
8. The method for decomposing tantalum-niobium slurry according to claim 5, wherein the hazard eliminating operation is performed based on process parameters, and specifically comprises:
setting preset values for each parameter of temperature, pressure and liquid level change rate;
and when the real-time value of any one parameter of the temperature, the pressure and the liquid level change rate reaches the preset value of the process parameter, carrying out danger elimination operation, wherein the danger elimination operation comprises one or more of reducing the acid liquor conveying rate, stopping acid liquor conveying, conveying danger elimination process water and stopping danger elimination process water conveying.
9. The method of decomposing tantalum-niobium slurry as claimed in claim 8, wherein:
setting three preset values for each parameter of temperature, pressure and liquid level change rate, wherein the three preset values are respectively a speed reduction preset value, an acid stopping preset value and an acid stopping and water adding preset value, and the speed reduction preset value, the acid stopping preset value and the acid stopping and water adding preset value are sequentially increased;
when the real-time value of any one parameter of the temperature, the pressure and the liquid level change rate reaches the deceleration preset value of the process parameter, the acid liquor conveying rate is reduced;
when the real-time value of any one parameter of the temperature, the pressure and the liquid level change rate reaches the acid stop preset value of the process parameter, stopping acid liquor conveying;
and when the real-time value of any parameter of the temperature, the pressure and the liquid level change rate reaches the preset acid-stopping and water-adding value of the process parameter, stopping acid liquor conveying and conveying dangerous process water.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3972710A (en) * | 1974-07-23 | 1976-08-03 | Hermann C. Starchk Berlin | Method of upgrading tantalum and niobium concentration in slags |
| JP2010196125A (en) * | 2009-02-26 | 2010-09-09 | Sumitomo Metal Mining Co Ltd | Method for leaching copper raw material containing copper sulfide mineral |
| CN113801995A (en) * | 2020-06-12 | 2021-12-17 | 稀美资源(广东)有限公司 | Intelligent control device for shaftless spiral continuous feeding of tantalum-niobium alloy ore |
| CN216038730U (en) * | 2021-09-28 | 2022-03-15 | 锦益创典(天津)科技有限责任公司 | Tantalum-niobium extraction residual liquid treatment system |
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- 2023-02-13 CN CN202310100972.7A patent/CN115852172B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3972710A (en) * | 1974-07-23 | 1976-08-03 | Hermann C. Starchk Berlin | Method of upgrading tantalum and niobium concentration in slags |
| JP2010196125A (en) * | 2009-02-26 | 2010-09-09 | Sumitomo Metal Mining Co Ltd | Method for leaching copper raw material containing copper sulfide mineral |
| CN113801995A (en) * | 2020-06-12 | 2021-12-17 | 稀美资源(广东)有限公司 | Intelligent control device for shaftless spiral continuous feeding of tantalum-niobium alloy ore |
| CN216038730U (en) * | 2021-09-28 | 2022-03-15 | 锦益创典(天津)科技有限责任公司 | Tantalum-niobium extraction residual liquid treatment system |
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