CN113699388A - Tungsten waste material decomposition process selection system - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 196
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 200
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- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 15
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
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- 229910017052 cobalt Inorganic materials 0.000 claims description 5
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
- C22B34/365—Obtaining tungsten from spent catalysts
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Abstract
The invention relates to the field of rare metal separation science, and provides a tungsten waste decomposition process selection system which comprises the steps of tungsten waste property analysis, tungsten waste decomposition process selection, tungsten waste decomposition process execution, tungsten waste utilization process evaluation feedback, tungsten waste utilization process optimization and correction, tungsten waste property and decomposition process database and the like. The method comprises the steps of firstly analyzing the properties of the tungsten waste, formulating a tungsten waste decomposition process according to an analysis result, then executing the tungsten waste decomposition process, then carrying out evaluation feedback according to the process execution condition, then optimizing and correcting the original process, and finally warehousing and storing the properties of the tungsten waste and the decomposition process. The tungsten waste decomposition process selection system can rapidly analyze the properties of the tungsten waste, and performs execution, feedback, optimization and correction through the selection process to finally form a tungsten waste property and decomposition process database.
Description
Technical Field
The invention relates to the field of rare metal separation science, in particular to a tungsten waste decomposition process selection system.
Background
The tungsten-molybdenum waste refers to decomposition slag, waste water sludge and molybdenum removal slag generated in the tungsten-molybdenum smelting process, and waste materials generated in the tungsten-molybdenum product processing or utilizing process, such as waste hard alloy, waste grinding material, waste tungsten stranded wire, waste catalyst and the like, and is rich in WO3And valuable metals such as Mo, Cu, Fe, Co, Ni, Mn, etc. With the exhaustion of high-quality tungsten-molybdenum mineral resources, tungsten-molybdenum waste materials have become very important secondary metal resources. At present, aiming at the problem of difficult resource utilization of tungsten and molybdenum wastes, a great deal of technical research and development work is carried out, some important progress is made, but the technical bottleneck still exists. The most critical problem is that: the tungsten-molybdenum waste materials are various in variety, and how to establish a set of efficient and accurate identification and classification system and a decomposition process selection system is the primary problem influencing the utilization rate of various tungsten-molybdenum waste materials.
Aiming at the problem of low efficiency of tungsten waste process selection, the technology of the invention establishes a decomposition process selection system, which comprises the steps of tungsten waste property analysis, tungsten waste decomposition process selection, tungsten waste decomposition process execution, tungsten waste utilization process evaluation feedback, tungsten waste utilization process optimization and correction, tungsten waste property and decomposition process database, and provides a system technology for realizing accurate judgment and efficient selection of the tungsten waste decomposition process.
Disclosure of Invention
The invention aims to provide a tungsten waste decomposition process selection system, which is mainly used for solving the problems of low process selection efficiency and no system guidance method of tungsten waste due to various types.
The technical problem of the invention is mainly solved by the following technical scheme: the method comprises the following steps:
(1) analyzing the properties of the tungsten waste: firstly, classifying and analyzing the tungsten waste, namely, refractory mineral tungsten-like waste, high-barium scheelite, high-molybdenum scheelite, high-silicon scheelite, high-calcium scheelite, high-phosphorus scheelite, high-tin scheelite and synthetic scheelite, detecting the contents of tungsten, barium, calcium, molybdenum, silicon, phosphorus and tin elements in the waste, and evaluating the decomposition performance of the mineral; secondly, refractory waste slag tungsten waste, high-grade tungsten smelting alkali decomposition slag, molybdenum removal slag, tungsten smelting waste water treatment tank sludge, feed liquid tank cleaning slag and tungsten-molybdenum-containing phosphorus removal slag are detected, the content of tungsten, molybdenum, calcium, sulfur and phosphorus elements is detected for the waste, and the mineral decomposition performance is evaluated; and thirdly, refractory tungsten-containing waste products, such as tungsten waste, waste catalysts, waste grinding materials, waste tungsten-containing electrical contacts and waste tungsten stranded wire and waste hard alloy are detected, the content of tungsten, molybdenum, cobalt, nickel and aluminum elements is detected, and the decomposition performance of the minerals is evaluated.
(2) The tungsten waste decomposition process comprises the following steps: according to the tungsten waste property analysis result and the selection decomposition process in the step (1), the selection principle is that firstly, the mineral tungsten waste which is difficult to smelt contains high barium (barium is more than or equal to 0.5 percent), high tin (tin is more than or equal to 5 percent), high calcium (calcium is more than or equal to 12 percent) and high-silicon scheelite (silicon is more than or equal to 5 percent), and a sodium carbonate high-pressure decomposition process is selected; selecting a roasting-sodium carbonate high-pressure decomposition process for scheelite containing high molybdenum (molybdenum is more than or equal to 2%) and high phosphorus (phosphorus is more than or equal to 1%); highly synthesizing scheelite (tungsten trioxide is more than or equal to 40 percent) and selecting a concentrated hydrochloric acid direct decomposition process; synthesizing the white tungsten with low degree (more than or equal to 5 percent and less than 40 percent of tungsten trioxide), and selecting dilute hydrochloric acid pretreatment-concentrated hydrochloric acid decomposition process. Secondly, refractory waste slag tungsten waste, high-grade tungsten smelting alkali decomposition slag (tungsten trioxide is more than or equal to 2%), sludge of a tungsten smelting waste water treatment tank (tungsten trioxide is more than or equal to 2%), feed liquid clear tank slag (tungsten trioxide is more than or equal to 2%), phosphorus removal slag containing tungsten and molybdenum (tungsten trioxide is more than or equal to 2%), and a sodium carbonate high-pressure decomposition process is selected; the molybdenum removing slag is selected from a sodium hydroxide low-pressure decomposition process. Thirdly, selecting an oxidizing roasting-sodium carbonate high-pressure decomposition process for tungsten-like waste materials and waste catalysts which are difficult to smelt tungsten-containing waste products; selecting a roasting oxidation-sodium hydroxide medium-pressure decomposition process for the waste grinding material; the waste tungsten-containing electrical contact, the waste tungsten stranded wire and the waste hard alloy are treated by a crushing-oxidation-sodium hydroxide decomposition process. The tungsten waste decomposition process is selected and then the next step is carried out.
(3) The tungsten waste utilization process is implemented as follows: after the decomposition process is selected in the step (2), a detailed process execution is formulated, wherein the process execution principle is that firstly, the mineral tungsten waste which is difficult to smelt contains high barium (barium is more than or equal to 0.5 percent), high tin (tin is more than or equal to 5 percent), high calcium (calcium is more than or equal to 12 percent) and high silicon scheelite (silicon is more than or equal to 5 percent), and the high-pressure decomposition process of sodium carbonate is characterized in that the liquid-solid ratio is controlled to be more than or equal to 3:1, the concentration of sodium carbonate is controlled to be less than or equal to 180g/L, and the decomposition pressure is controlled to be less than or equal to 22 Mpa; scheelite containing high molybdenum (more than or equal to 2 percent) and high phosphorus (more than or equal to 1 percent), a roasting-sodium carbonate high-pressure decomposition process, wherein the roasting temperature is less than or equal to 600 ℃, the sodium carbonate high pressure is realized, the liquid-solid ratio is controlled to be more than or equal to 3:1, the sodium carbonate concentration is controlled to be less than or equal to 180g/L, and the decomposition pressure is controlled to be less than or equal to 22 Mpa; highly synthesizing scheelite (tungsten trioxide is more than or equal to 40 percent), selecting a concentrated hydrochloric acid direct decomposition process, wherein the hydrochloric acid concentration at the decomposition end is more than or equal to 4.5mol/L, and the decomposition temperature is 95-100 ℃; synthesizing the scheelite with low degree (more than or equal to 5 percent and less than 40 percent of tungsten trioxide), selecting a dilute hydrochloric acid pretreatment-concentrated hydrochloric acid decomposition process, wherein the hydrochloric acid concentration at the end of pretreatment is more than or equal to 1.1mol/L at 1.5mol/L and the hydrochloric acid concentration at the end of decomposition is more than or equal to 4.5mol/L, the pretreatment time is more than or equal to 50min, the decomposition time is more than or equal to 50min, and the decomposition temperature is 95-100 ℃. Secondly, refractory waste slag tungsten waste, high-grade tungsten smelting alkali decomposition slag (tungsten trioxide is more than or equal to 2 percent), tungsten smelting waste water treatment tank sludge (tungsten trioxide is more than or equal to 2 percent), feed liquid clear tank slag (tungsten trioxide is more than or equal to 2 percent), tungsten-molybdenum-containing phosphorus removal slag (tungsten trioxide is more than or equal to 2 percent), selecting a sodium carbonate high-pressure decomposition process, controlling the liquid-solid ratio to be more than or equal to 3:1, controlling the concentration of sodium carbonate to be less than or equal to 180g/L, and controlling the decomposition pressure to be less than or equal to 2.2 Mpa; the molybdenum removing slag is selected by a sodium hydroxide low-pressure decomposition process, the liquid-solid ratio is controlled to be more than or equal to 1:1 and is more than or equal to 2:1, the decomposition pressure is controlled to be less than or equal to 0.5Mpa, and the concentration of the sodium hydroxide is controlled to be less than or equal to 450 g/L. Thirdly, selecting an oxidation roasting-sodium carbonate high-pressure decomposition process for tungsten wastes and waste catalysts which are difficult to smelt tungsten-containing waste products, wherein the roasting temperature is controlled to be more than or equal to 600 ℃ and less than or equal to 800 ℃, the sodium carbonate is decomposed under high pressure, the liquid-solid ratio is controlled to be more than or equal to 3:1, the concentration of the sodium carbonate is controlled to be less than or equal to 180g/L, and the decomposition pressure is controlled to be less than or equal to 22 Mpa; selecting a roasting oxidation-sodium hydroxide medium-pressure decomposition process for the waste grinding material, wherein the roasting temperature is controlled to be more than or equal to 300 ℃ and less than or equal to 500 ℃, the liquid-solid ratio is controlled to be more than or equal to 2:1, the concentration of sodium hydroxide is controlled to be less than or equal to 450g/L, and the decomposition pressure is controlled to be less than or equal to 0.5 Mpa; the waste tungsten-containing electrical contact and the waste tungsten-containing twisted wire are treated by a crushing-roasting oxidation/hot acid leaching oxidation-sodium hydroxide decomposition process, the crushing and the reinforced crushing are carried out, the proportion of minus 325 meshes is more than or equal to 95 percent, the roasting oxidation is carried out, the temperature is more than or equal to 700 ℃ and less than or equal to 1100 ℃, the hot acid leaching oxidation is carried out, the solid-to-solid ratio of a sodium hydroxide decomposition liquid is controlled to be more than or equal to 2:1, the concentration of the sodium hydroxide decomposition end point is controlled to be more than or equal to 50g/L, the decomposition is carried out at normal pressure, and the decomposition temperature is more than or equal to 90 ℃ and less than or equal to 100 ℃.
(4) Tungsten waste decomposition process evaluation feedback: after the process execution in the step (3) is completed, the evaluation feedback is carried out on the process execution result, and the evaluation feedback principle is that firstly, the refractory mineral tungsten waste contains high barium (barium is more than or equal to 0.5%), high tin (tin is more than or equal to 5%), high calcium (calcium is more than or equal to 12%) and high silicon scheelite (silicon is more than or equal to 5%); the method comprises the following steps of (1%) roasting-sodium carbonate high-pressure decomposition of scheelite containing high molybdenum (molybdenum is more than or equal to 2%) and high phosphorus (phosphorus is more than or equal to 1%), wherein the content of tungsten trioxide in decomposed slag is less than or equal to 0.5%, the leaching is excellent, the content of tungsten trioxide in decomposed slag is more than 0.5%, the leaching is good, the content of tungsten trioxide in decomposed slag is more than 1%, and the leaching is poor; highly synthesizing scheelite (the content of tungsten trioxide is more than or equal to 40 percent), selecting a concentrated hydrochloric acid direct decomposition process, wherein the content of tungsten trioxide in tungstic acid is more than or equal to 90 percent, the leaching is excellent, the content of tungsten trioxide in tungstic acid is more than or equal to 80 percent, the leaching is good, the content of tungsten trioxide in tungstic acid is less than 80 percent, and the decomposition is poor; synthesizing low-degree scheelite (tungsten trioxide is more than or equal to 10% and less than 40%), selecting a dilute hydrochloric acid pretreatment-concentrated hydrochloric acid decomposition process, wherein tungsten trioxide in tungstic acid is more than or equal to 85%, the leaching quality is excellent, the content of tungsten trioxide in tungstic acid is more than or equal to 75%, the leaching quality is good, the content of tungsten trioxide in tungstic acid is less than 75%, and the decomposition is poor. Secondly, refractory waste slag tungsten waste, high tungsten smelting alkali decomposition slag (tungsten trioxide is more than or equal to 2%), sludge of a tungsten smelting waste water treatment tank (tungsten trioxide is more than or equal to 2%), feed liquid clear tank slag (tungsten trioxide is more than or equal to 2%), phosphorus removal slag containing tungsten and molybdenum (tungsten trioxide is more than or equal to 2%), a sodium carbonate high-pressure decomposition process is selected, the content of tungsten trioxide in decomposition slag is less than or equal to 0.5%, the leaching quality is excellent, the content of tungsten trioxide in decomposition slag is more than or equal to 0.5%, the leaching quality is good, the content of tungsten trioxide in decomposition slag is more than 1%, and the leaching difference is poor; the molybdenum removing slag is prepared by a sodium hydroxide low-pressure decomposition process, the content of tungsten trioxide in the decomposition slag is less than or equal to 0.5%, the leaching is excellent, the content of tungsten trioxide in the decomposition slag is more than or equal to 0.5% in 1%, the leaching is good, the content of tungsten trioxide in the decomposition slag is more than 1%, and the leaching difference is poor. Thirdly, selecting a carbonic acid roasting-high pressure decomposition process to smelt the tungsten-like waste materials and waste catalysts which are difficult to smelt and contain tungsten waste products, wherein the content of tungsten trioxide in the decomposition slag is less than or equal to 0.5 percent, the leaching is excellent, the content of tungsten trioxide in the decomposition slag is more than or equal to 1 percent and is more than 0.5 percent, the leaching is good, the content of tungsten trioxide in the decomposition slag is more than 1 percent, and the leaching is poor; selecting a roasting oxidation-sodium hydroxide medium-pressure decomposition process for the waste grinding material, wherein the content of tungsten trioxide in decomposition slag is less than or equal to 0.5%, the leaching is excellent, the content of tungsten trioxide in decomposition slag is more than or equal to 0.5% in 1%, the leaching is good, the content of tungsten trioxide in decomposition slag is more than 1%, and the leaching is poor; the waste tungsten-containing electrical contact and the waste tungsten-containing skein are treated by a crushing-roasting oxidation/hot acid leaching oxidation-sodium hydroxide decomposition process, the content of tungsten trioxide in decomposition slag is less than or equal to 0.5%, the leaching is excellent, the content of tungsten trioxide in decomposition slag is more than 0.5% in 1% or more, the leaching is good, the content of tungsten trioxide in decomposition slag is more than 1%, and the leaching is poor.
(5) Optimizing and correcting the tungsten waste decomposition process: the evaluation of the decomposition process is fed back through the step (4), and the decomposition process is optimized and corrected according to the principle that firstly, the refractory mineral tungsten waste is leached out optimally, the process parameters are directly filed for later use, and the incoming materials are processed according to the process; leaching well, and continuously optimizing technological parameters; the leaching difference and the process are replaced, and the investigation is continued; secondly, the refractory waste slag tungsten waste is leached out optimally, the technological parameters are directly filed for later use, and the incoming materials are treated according to the process; leaching well, and continuously optimizing technological parameters; the leaching difference and the process are replaced, tungsten wastes such as the difficult-to-smelt tungsten-containing waste products are continuously inspected, the leaching is excellent, the process parameters are directly filed for standby, and the incoming materials are processed according to the process; leaching well, and continuously optimizing technological parameters; and (5) changing the process and continuing to examine the leaching difference.
(6) Establishing a tungsten waste property and decomposition process database: the system data is classified and stored, the original records are placed and stored in a standard mode, and meanwhile, electronic files are manufactured for future reference, so that complete and reliable data are provided for accurate judgment and efficient selection of the subsequent tungsten-molybdenum waste decomposition process.
The invention has the beneficial effects that: through analysis of tungsten waste material properties, selection of a tungsten waste material decomposition process, execution of the tungsten waste material decomposition process, evaluation feedback of the tungsten waste material utilization process, optimization and correction of the tungsten waste material utilization process, classification of the tungsten waste materials and formulation of a decomposition process database, the tungsten waste materials are classified quickly and accurately, and the aim of efficiently treating the tungsten waste materials is fulfilled.
Drawings
FIG. 1 is a process flow diagram of the present invention;
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments and the accompanying drawings.
Example 1
Example the raw material used was from a tungsten molybdenum ore dressing site in shanxi.
(1) Analyzing the properties of the tungsten waste: the method comprises the steps of classifying tungsten waste, detecting the contents of tungsten, barium, calcium, molybdenum, silicon, phosphorus and tin in the tungsten waste, wherein the tungsten waste belongs to refractory mineral tungsten waste, the detection results comprise 23.50% of tungsten, 3.62% of barium, 12.50% of calcium, 0.2% of molybdenum, 6.21% of silicon, 0.12% of phosphorus and 0.36% of tin, and the detection data show that the raw materials belong to high-barium high-silicon low-grade scheelite, the property analysis of the tungsten waste is completed, and the next step is carried out.
(2) The tungsten waste decomposition process comprises the following steps: and (2) according to the tungsten waste property analysis result in the step (1), referring to the principle of the selected decomposition process, preferentially selecting a roasting-sodium carbonate high-pressure decomposition process for treatment, and then entering the next step.
(3) The tungsten waste decomposition process is implemented as follows: after the roasting-sodium carbonate high-pressure decomposition process is selected in the step (2), detailed process execution is formulated, the process execution principle is that the roasting temperature is 500 ℃, the sodium carbonate high-pressure decomposition is carried out, the liquid-solid ratio is controlled to be 4:1, the concentration of the sodium carbonate is controlled to be 160g/L, the decomposition pressure is controlled to be 1.8Mpa, the decomposition process is completed, the decomposition slag is filtered, washed, dried and weighed, a sample is prepared, the content of tungsten trioxide is detected, and then the next step is carried out.
(4) Tungsten waste decomposition process evaluation feedback: and (4) after the process execution in the step (3) is finished, evaluating and feeding back the process execution result, wherein the evaluation feedback principle is that firstly, the content of the tungsten trioxide in the decomposition residue is less than or equal to 0.5%, the leaching is excellent, 1% or more of the tungsten trioxide in the decomposition residue is more than 0.5%, the leaching is good, the content of the tungsten trioxide in the decomposition residue is more than 1%, and the leaching is poor. The detection result of the actual decomposition slag is 0.35 percent of tungsten trioxide, and the evaluation feedback of the decomposition process is excellent. And then proceed to the next step.
(5) Optimizing and correcting the tungsten waste decomposition process: and (4) evaluating and feeding back the decomposition process through the step (4), and optimizing and correcting the decomposition process according to the optimization and correction principle that firstly, the refractory mineral tungsten waste is leached out optimally, and the process parameters are directly filed for later use, and then the next step is carried out.
(6) Establishing a tungsten waste property and decomposition process database: the method comprises the steps of recording the production area, the property analysis data and the decomposition process data of the high-barium high-silicon scheelite, classifying and storing the scheelite system, storing the scheelite system in a standard mode through original records, manufacturing electronic files for future reference, and providing complete and reliable data for accurate judgment and efficient selection of the subsequent waste selecting and decomposing process.
Example 2
Example synthetic white tungsten from a byproduct of a tin field in much greater amounts in the west and the river was used as a raw material.
(1) Analyzing the properties of the tungsten waste: the method comprises the steps of classifying tungsten waste, detecting the contents of tungsten, barium, calcium, molybdenum, silicon, phosphorus and tin in the tungsten waste, wherein the tungsten waste belongs to refractory mineral tungsten waste, the detection results comprise 56.20% of tungsten, 18.30% of calcium, 3.25% of molybdenum, 0.1% of silicon, 0.12% of phosphorus and 0.16% of tin, and the detection data show that the tungsten waste belongs to high-calcium synthetic white tungsten, the property analysis of the tungsten waste is completed, and the next step is carried out.
(2) The tungsten waste decomposition process comprises the following steps: and (2) according to the tungsten waste material property analysis result in the step (1), referring to the principle of the selected decomposition process, preferentially selecting a concentrated hydrochloric acid direct decomposition process for treatment, and then entering the next step.
(3) The tungsten waste decomposition process is implemented as follows: after the step (2), selecting a concentrated hydrochloric acid direct decomposition process, making a detailed process execution, wherein the process execution principle is that the concentration of hydrochloric acid at the decomposition end point is more than or equal to 4.5mol/L, the decomposition temperature is 95-100 ℃, the decomposition process execution is completed, the decomposition slag is filtered, washed, dried, weighed, sample preparation is carried out, the content of tungsten trioxide is detected, and then the next step is carried out.
(4) Tungsten waste decomposition process evaluation feedback: and (4) after the process execution in the step (3) is finished, evaluating and feeding back the process execution result, wherein the evaluation feedback principle is that firstly, the mineral tungsten-like waste is difficult to smelt, tungsten trioxide in tungstic acid is more than or equal to 90%, the leaching is excellent, the content of tungsten trioxide in tungstic acid is more than or equal to 80%, the leaching is good, the content of tungsten trioxide in tungstic acid is less than 80%, and the decomposition is poor. The detection results of the actual decomposition slag are 93.10% of tungsten trioxide and 0.89% of molybdenum, and the evaluation feedback of the decomposition process is excellent. And then proceed to the next step.
(5) Optimizing and correcting the tungsten waste decomposition process: and (4) evaluating and feeding back the decomposition process through the step (4), and optimizing and correcting the decomposition process according to the principle that firstly, the refractory mineral tungsten waste is decomposed well, and the process parameters are directly filed for later use, and then the next step is carried out.
(6) Establishing a tungsten waste property and decomposition process database: the production place, the property analysis data and the decomposition process data of the high-calcium high-molybdenum synthetic scheelite are recorded, the system is classified and stored, the original records are placed and stored in a standard mode, meanwhile, an electronic file is made for future reference, and complete and reliable data are provided for accurate judgment and efficient selection of the subsequent waste selecting and decomposing process.
Example 3
Examples tungsten containing abrasives were used by a company of ningxiang of Hunan.
(1) Analyzing the properties of the tungsten waste: firstly, classifying the tungsten waste, belonging to the waste tungsten-containing grinding material, detecting the contents of tungsten, cobalt and molybdenum elements in the waste, wherein the detection results comprise 87.20% of tungsten, 5.35% of cobalt and 0.1% of molybdenum, and the detection data show that the raw materials belong to the waste grinding material containing tungsten and cobalt, the property analysis of the tungsten waste is completed, and the next step is carried out.
(2) The tungsten waste decomposition process comprises the following steps: and (2) according to the tungsten waste property analysis result in the step (1), referring to the principle of an optional decomposition process, preferentially selecting a roasting oxidation-sodium hydroxide medium-pressure decomposition process for treatment, and then entering the next step.
(3) The tungsten waste decomposition process is implemented as follows: after a roasting oxidation-sodium hydroxide medium-pressure decomposition process is selected in the step (2), detailed process execution is formulated, wherein the process execution principle is that the roasting temperature is controlled to be 350 ℃, the sodium hydroxide medium-pressure leaching is carried out, the liquid-solid ratio is controlled to be 2:1, the concentration of the sodium hydroxide is controlled to be 400g/L, the decomposition pressure is controlled to be 0.5Mpa, the decomposition process is completed, the decomposition slag is filtered, washed, dried, weighed, sample preparation is carried out, the content of tungsten trioxide is detected, and then the next step is carried out.
(4) Tungsten waste decomposition process evaluation feedback: and (4) after the process execution in the step (3) is finished, evaluating and feeding back the process execution result, wherein the evaluation feedback principle is that the content of the tungsten trioxide in the decomposition residue is less than or equal to 0.5%, the leaching quality is excellent, the content of the tungsten trioxide in the decomposition residue is more than or equal to 0.5%, the leaching quality is good, the content of the tungsten trioxide in the decomposition residue is more than 1%, and the leaching difference is poor. The actual detection result of the decomposed slag is 6.0% of tungsten trioxide, and the evaluation feedback of the decomposition process is poor. And then proceed to the next step.
(5) Optimizing and correcting the tungsten waste decomposition process: and (4) evaluating and feeding back the decomposition process through the step (4), optimizing and correcting the decomposition process according to the principle that the refractory mineral tungsten waste is poor in decomposition, optimizing and correcting the process, secondarily roasting decomposition slag, mixing the decomposition slag with sodium carbonate, roasting, controlling the temperature to be 350 ℃, adding 10% of the sodium carbonate, carrying out low-alkali secondary leaching after roasting, controlling the concentration of sodium hydroxide to be 80-100 g/L and the leaching pressure to be 0.3MPa, completing leaching, filtering, washing, drying and weighing leaching slag, preparing a sample, measuring the content of WO3 to be 0.42%, and obtaining an excellent leaching effect. The decomposition process is optimized and modified to roasting oxidation, sodium hydroxide medium-pressure leaching, high-slag secondary sodium carbonate roasting leaching and low-alkali medium-pressure leaching. And then proceed to the next step.
(6) Establishing a tungsten waste property and decomposition process database: the production place, the property analysis data and the decomposition process data of the waste grinding material are recorded, the system is classified and stored, the original records are stored in a standard mode, meanwhile, electronic files are manufactured for future reference, and complete and reliable data are provided for accurate judgment and efficient selection of the subsequent waste selecting and decomposing process.
The above examples are merely representative of preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (1)
1. A tungsten waste material decomposition process selection system is characterized by comprising the following steps:
(1) analyzing the properties of the tungsten waste: firstly, classifying and analyzing the tungsten waste, namely, refractory mineral tungsten-like waste, high-barium scheelite, high-molybdenum scheelite, high-silicon scheelite, high-calcium scheelite, high-phosphorus scheelite, high-tin scheelite and synthetic scheelite, detecting the contents of tungsten, barium, calcium, molybdenum, silicon, phosphorus and tin elements in the waste, and evaluating the decomposition performance of the mineral; secondly, refractory waste slag tungsten waste, high-grade tungsten smelting alkali decomposition slag, molybdenum removal slag, tungsten smelting waste water treatment tank sludge, feed liquid tank cleaning slag and tungsten-molybdenum-containing phosphorus removal slag are detected, the content of tungsten, molybdenum, calcium, sulfur and phosphorus elements is detected for the waste, and the mineral decomposition performance is evaluated; thirdly, difficult-to-smelt tungsten-containing waste products, such as tungsten waste, waste catalysts, waste grinding materials, waste tungsten-containing electrical contacts and waste tungsten stranded wire and waste hard alloy, detecting the content of tungsten, molybdenum, cobalt, nickel and aluminum elements, and evaluating the decomposition performance of the minerals;
(2) the tungsten waste decomposition process comprises the following steps: according to the tungsten waste property analysis result and the selection decomposition process in the step (1), the selection principle is that firstly, the mineral tungsten waste which is difficult to smelt contains high barium (barium is more than or equal to 0.5 percent), high tin (tin is more than or equal to 5 percent), high calcium (calcium is more than or equal to 12 percent) and high-silicon scheelite (silicon is more than or equal to 5 percent), and a sodium carbonate high-pressure decomposition process is selected; selecting a roasting-sodium carbonate high-pressure decomposition process for scheelite containing high molybdenum (molybdenum is more than or equal to 2%) and high phosphorus (phosphorus is more than or equal to 1%); highly synthesizing scheelite (tungsten trioxide is more than or equal to 40 percent) and selecting a concentrated hydrochloric acid direct decomposition process; synthesizing low-degree scheelite (tungsten trioxide is more than or equal to 5% and less than 40%), and selecting dilute hydrochloric acid pretreatment-concentrated hydrochloric acid decomposition process; secondly, refractory waste slag tungsten waste, high-grade tungsten smelting alkali decomposition slag (tungsten trioxide is more than or equal to 2%), sludge of a tungsten smelting waste water treatment tank (tungsten trioxide is more than or equal to 2%), feed liquid clear tank slag (tungsten trioxide is more than or equal to 2%), phosphorus removal slag containing tungsten and molybdenum (tungsten trioxide is more than or equal to 2%), and a sodium carbonate high-pressure decomposition process is selected; selecting a sodium hydroxide low-pressure decomposition process for molybdenum removal slag; thirdly, selecting an oxidizing roasting-sodium carbonate high-pressure decomposition process for tungsten-like waste materials and waste catalysts which are difficult to smelt tungsten-containing waste products; selecting a roasting oxidation-sodium hydroxide medium-pressure decomposition process for the waste grinding material; selecting a crushing-oxidizing-sodium hydroxide decomposing process to treat the waste tungsten-containing electrical contact, the waste tungsten stranded wire and the waste hard alloy; the tungsten waste decomposition process is selected, and then the next step is carried out;
(3) the tungsten waste decomposition process is implemented as follows: after the decomposition process is selected in the step (2), a detailed process execution is formulated, wherein the process execution principle is that firstly, the mineral tungsten waste which is difficult to smelt contains high barium (barium is more than or equal to 0.5%), high tin (tin is more than or equal to 5%), high calcium (calcium is more than or equal to 12%), high-silicon scheelite (silicon is more than or equal to 5%), a sodium carbonate high-pressure decomposition process is carried out, the liquid-solid ratio is controlled to be more than or equal to 3:1, the concentration of sodium carbonate is controlled to be less than or equal to 180g/L, and the decomposition pressure is controlled to be less than or equal to 2.2 Mpa; scheelite containing high molybdenum (more than or equal to 2 percent) and high phosphorus (more than or equal to 1 percent), a roasting-sodium carbonate high-pressure decomposition process, wherein the roasting temperature is less than or equal to 600 ℃, the sodium carbonate high pressure is realized, the liquid-solid ratio is controlled to be more than or equal to 3:1, the sodium carbonate concentration is controlled to be less than or equal to 180g/L, and the decomposition pressure is controlled to be less than or equal to 22 Mpa; highly synthesizing scheelite (tungsten trioxide is more than or equal to 40 percent), selecting a concentrated hydrochloric acid direct decomposition process, wherein the hydrochloric acid concentration at the decomposition end is more than or equal to 4.5 mol/L; synthesizing scheelite with low degree (more than or equal to 5 percent and less than 40 percent of tungsten trioxide), selecting a dilute hydrochloric acid pretreatment-concentrated hydrochloric acid decomposition process, wherein 1.5mol/L is more than or equal to 1.1mol/L of hydrochloric acid at the end of pretreatment, the concentration of hydrochloric acid at the end of decomposition is more than or equal to 4.5mol/L, the pretreatment time is more than or equal to 50min, and the decomposition time is more than or equal to 50 min; secondly, refractory waste slag tungsten waste, high-grade tungsten smelting alkali decomposition slag (tungsten trioxide is more than or equal to 2 percent), tungsten smelting waste water treatment tank sludge (tungsten trioxide is more than or equal to 2 percent), feed liquid clear tank slag (tungsten trioxide is more than or equal to 2 percent), tungsten-molybdenum-containing phosphorus removal slag (tungsten trioxide is more than or equal to 2 percent), selecting a sodium carbonate high-pressure decomposition process, controlling the liquid-solid ratio to be more than or equal to 3:1, controlling the concentration of sodium carbonate to be less than or equal to 180g/L, and controlling the decomposition pressure to be less than or equal to 2.2 Mpa; selecting a sodium hydroxide low-pressure decomposition process for molybdenum removal slag, wherein the liquid-solid ratio is more than or equal to 2:1 and is more than or equal to 1:1, the decomposition pressure is less than or equal to 0.5Mpa, and the concentration of sodium hydroxide is less than or equal to 450 g/L; thirdly, selecting an oxidation roasting-sodium carbonate high-pressure decomposition process for tungsten wastes and waste catalysts which are difficult to smelt tungsten-containing waste products, wherein the roasting temperature is controlled to be more than or equal to 600 ℃ and less than or equal to 800 ℃, the sodium carbonate is decomposed under high pressure, the liquid-solid ratio is controlled to be more than or equal to 3:1, the concentration of the sodium carbonate is controlled to be less than or equal to 180g/L, and the decomposition pressure is controlled to be less than or equal to 2.2 Mpa; selecting a roasting oxidation-sodium hydroxide medium-pressure decomposition process for the waste grinding material, controlling the roasting temperature to be more than or equal to 300 ℃ and less than or equal to 500 ℃, controlling the using amount of sodium carbonate, controlling the liquid-solid ratio to be more than or equal to 2:1, controlling the concentration of sodium hydroxide to be less than or equal to 450g/L, and controlling the decomposition pressure to be less than or equal to 0.5Mpa, wherein the using amount of sodium carbonate is more than or equal to 5% and less than or equal to 10%; selecting a crushing-roasting oxidation/hot acid leaching oxidation-sodium hydroxide decomposition process for treating the waste tungsten-containing electrical contact and the waste tungsten-containing twisted wire, crushing, strengthening crushing, wherein the proportion of minus 325 meshes is more than or equal to 95%, roasting oxidation is carried out, the temperature is more than or equal to 700 ℃ and less than or equal to 1100 ℃, hot acid leaching oxidation is carried out, the solid-to-solid ratio of a sodium hydroxide decomposition liquid is controlled to be more than or equal to 2:1, the concentration of the sodium hydroxide decomposition end point is controlled to be more than or equal to 50g/L, normal pressure decomposition is carried out, and the decomposition temperature is more than or equal to 90 ℃ and less than or equal to 100 ℃;
(4) tungsten waste decomposition process evaluation feedback: after the process execution is completed in the step (3), the result of the process execution is evaluated and fed back, and the evaluation feedback principle is that firstly, the refractory mineral tungsten-like waste contains high-barium (barium is more than or equal to 0.5%), high-tin (tin is more than or equal to 5%), high-calcium (calcium is more than or equal to 12%), high-silicon scheelite (silicon is more than or equal to 5%), high-molybdenum (molybdenum is more than or equal to 2%) and high-phosphorus (phosphorus is more than or equal to 1%), a roasting-sodium carbonate high-pressure decomposition process is selected, the content of the decomposed slag tungsten trioxide is less than or equal to 0.5%, the leaching is excellent, the content of the 1% or more of the decomposed slag tungsten trioxide is more than 0.5%, the leaching is good, the content of the decomposed slag tungsten trioxide is more than 1%, and the leaching difference is high; highly synthesizing scheelite (the content of tungsten trioxide is more than or equal to 40 percent), selecting a concentrated hydrochloric acid direct decomposition process, wherein the content of tungsten trioxide in tungstic acid is more than or equal to 90 percent, the leaching is excellent, the content of tungsten trioxide in tungstic acid is more than or equal to 80 percent, the leaching is good, the content of tungsten trioxide in tungstic acid is less than 80 percent, and the decomposition is poor; synthesizing low-degree scheelite (tungsten trioxide is more than or equal to 10% and less than 40%), selecting a dilute hydrochloric acid pretreatment-concentrated hydrochloric acid decomposition process, wherein tungsten trioxide in tungstic acid is more than or equal to 85%, the leaching is excellent, the content of tungsten trioxide in tungstic acid is more than or equal to 75%, the leaching is good, the content of tungsten trioxide in tungstic acid is less than 75%, and the decomposition is poor; secondly, refractory waste slag tungsten waste, high tungsten smelting alkali decomposition slag (tungsten trioxide is more than or equal to 2%), sludge of a tungsten smelting waste water treatment tank (tungsten trioxide is more than or equal to 2%), feed liquid clear tank slag (tungsten trioxide is more than or equal to 2%), phosphorus removal slag containing tungsten and molybdenum (tungsten trioxide is more than or equal to 2%), a sodium carbonate high-pressure decomposition process is selected, the content of tungsten trioxide in decomposition slag is less than or equal to 0.5%, the leaching quality is excellent, the content of tungsten trioxide in decomposition slag is more than or equal to 0.5%, the leaching quality is good, the content of tungsten trioxide in decomposition slag is more than 1%, and the leaching difference is poor; a sodium hydroxide low-pressure decomposition process is selected for molybdenum removal slag, the content of tungsten trioxide in decomposition slag is less than or equal to 0.5%, the leaching is excellent, the content of tungsten trioxide in decomposition slag is more than or equal to 0.5% in 1%, the leaching is good, the content of tungsten trioxide in decomposition slag is more than 1%, and the leaching difference is poor; thirdly, selecting an oxidizing roasting-sodium carbonate high-pressure decomposition process to prepare tungsten-like waste materials and waste catalysts which are difficult to smelt and contain tungsten waste products, wherein the content of tungsten trioxide in decomposition residues is less than or equal to 0.5%, the leaching is excellent, the content of tungsten trioxide in decomposition residues is more than or equal to 0.5%, the leaching is good, the content of tungsten trioxide in decomposition residues is more than 1%, and the leaching difference is low; selecting a roasting oxidation-sodium hydroxide medium-pressure decomposition process for the waste grinding material, wherein the content of tungsten trioxide in decomposition slag is less than or equal to 0.5%, the leaching is excellent, the content of tungsten trioxide in decomposition slag is more than or equal to 0.5% in 1%, the leaching is good, the content of tungsten trioxide in decomposition slag is more than 1%, and the leaching is poor; the waste tungsten-containing electrical contact and the waste tungsten-containing skein are treated by a crushing-roasting oxidation/hot acid leaching oxidation-sodium hydroxide decomposition process, the content of tungsten trioxide in decomposition residue is less than or equal to 0.5%, the leaching is excellent, the content of tungsten trioxide in decomposition residue is more than 0.5% in 1% or more, the leaching is good, the content of tungsten trioxide in decomposition residue is more than 1%, and the leaching is poor;
(5) optimizing and correcting the tungsten waste decomposition process: the evaluation of the decomposition process is fed back through the step (4), and the decomposition process is optimized and corrected according to the principle that firstly, the refractory mineral tungsten waste is leached out optimally, the process parameters are directly filed for later use, and the incoming materials are processed according to the process; leaching well, and continuously optimizing technological parameters; the leaching difference and the process are replaced, and the investigation is continued; secondly, the refractory waste slag tungsten waste is leached out optimally, the technological parameters are directly filed for later use, and the incoming materials are treated according to the process; leaching well, and continuously optimizing technological parameters; the leaching difference and the process are replaced, and the investigation is continued; thirdly, the tungsten waste of the difficult-to-smelt tungsten-containing waste product is excellent in leaching, the technological parameters are directly filed for later use, and the incoming materials are processed according to the process; leaching well, and continuously optimizing technological parameters; the leaching difference and the process are replaced, and the investigation is continued;
(6) establishing a tungsten waste property and decomposition process database: the system data is classified and stored, the original records are placed and stored in a standard mode, and meanwhile, electronic files are manufactured for future reference, so that complete and reliable data are provided for accurate judgment and efficient selection of the subsequent tungsten-molybdenum waste decomposition process.
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