CN115007326B - Flotation method of high-calcium tungsten fluorite ore - Google Patents
Flotation method of high-calcium tungsten fluorite ore Download PDFInfo
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- CN115007326B CN115007326B CN202210356577.0A CN202210356577A CN115007326B CN 115007326 B CN115007326 B CN 115007326B CN 202210356577 A CN202210356577 A CN 202210356577A CN 115007326 B CN115007326 B CN 115007326B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
- B03D1/025—Froth-flotation processes adapted for the flotation of fines
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—Depressants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The application discloses a flotation method of high-calcium tungsten fluorite ore. For high calcium carbonate type tungsten fluorite ore, a combined inhibitor prepared by mixing oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch according to the mass ratio of 1-4:1-3:1-3 is adopted to inhibit scheelite, calcium carbonate and other gangue minerals, and the high-efficiency recovery of fluorite and tungsten is realized through a process of preferential fluorite flotation and tungsten flotation. The process is characterized in that the fluorite-scheelite flotation process is favorable for greatly improving the beneficiation index of fluorite and tungsten, reducing the beneficiation cost and the separation difficulty of tungsten flotation, and avoiding the problem that fluorite is difficult to recover after the fluorite is strongly restrained when scheelite flotation is performed preferentially; meanwhile, the fluorite flotation operation adopts a mode of adding different inhibitors in sections, so that the fluorite ore dressing index is improved, the subsequent tungsten recovery is facilitated, the grade and recovery rate of fluorite concentrate are both greatly improved, and the ore dressing cost is also correspondingly reduced.
Description
Technical Field
The application belongs to the technical field of flotation, and particularly relates to a flotation method of high-calcium tungsten fluorite ore.
Background
White tungsten is an important industrial raw material containing tungsten, and tungsten is widely applied to the fields of metallurgical machinery, petrochemical industry, aerospace, national defense and the like; fluorite is the most important fluorine-containing industrial raw material, and the fluorite can be widely applied to the fields of aerospace, medical and agricultural chemicals, mechano-electronics, air-conditioning refrigeration, corrosion prevention and fire extinguishment, atomic energy and the like. Both scheelite and fluorite have become important strategic mineral resources. The scheelite and fluorite resources in China are rich in reserves, but most of scheelite and fluorite resources are associated with the scheelite, and the scheelite and fluorite resources have low grade and complex components.
The conventional ore dressing method for scheelite-fluorite co-associated ore is a process of firstly floating scheelite preferentially and then recycling fluorite. At present, the industrial scheelite and fluorite flotation separation method is mainly a high-alkali method, namely, a large amount of sodium carbonate, sodium hydroxide, water glass and the like are added to control the pH value of ore pulp to be more than 12, scheelite is subjected to preferential flotation to inhibit fluorite, and then fluorite is subjected to flotation recovery from the tailings of the scheelite; in recent years, reports of a plurality of new processes, such as: (1) Tungsten and fluorite mixed flotation, and separating and flotation of fluorite and tungsten are carried out on the mixed concentrate; (2) The new technology for the preferential floatation of fluorite and the secondary floatation of tungsten is that a combined inhibitor is added under the weak acid or neutral condition to inhibit white tungsten, fluorite is preferentially floated, and then the white tungsten is activated and floated; (3) The metal-organic complex method is a process for preferentially floating tungsten and then floating fluorite.
The high-alkali method is to preferentially select scheelite, and a large amount of water glass is added under the high-alkali condition to strongly inhibit fluorite, so that the subsequent fluorite recovery is very difficult, the grade and recovery rate of fluorite concentrate are difficult to ensure, in addition, the water glass is large in dosage, the beneficiation wastewater is difficult to treat, and the beneficiation wastewater is difficult to recycle; the method has the advantages that the tungsten and fluorite are subjected to mixed flotation, and the mixed concentrate is subjected to a fluorite-tungsten separation flotation process, so that the recovery rate of tungsten can be greatly improved, but high-quality fluorite concentrate is difficult to obtain, and a large amount of water glass is required for separating the mixed concentrate, so that the problems that beneficiation wastewater is difficult to treat and difficult to recycle are also caused; the new process for preferential floatation of fluorite and re-floatation of scheelite can realize separation and recovery of scheelite and fluorite to a certain extent, but has similar problems as the high-alkali method, and when scheelite is strongly inhibited, a great amount of scheelite is lost in tailings; the metal-organic complex method is used for preferentially floating tungsten and re-floating fluorite, and the metal-organic complex has strong collecting capacity for scheelite and almost no collecting capacity for fluorite and calcite, so that fluorite is rarely lost in tungsten concentrate, and meanwhile, a large amount of inhibitors are not needed in tungsten flotation, thereby being beneficial to recovery of fluorite in subsequent fluorite flotation operation. However, the metal-organic complex method is a process for preferentially floating tungsten and then floating fluorite, so that the problems of large using amount of a collector and cost of a floating agent exist, and the metal-organic complex does not have strong collecting capacity for scheelite in all ores.
Patent number CN104084315A discloses that the target mineral is completely dissociated by one-time grinding, usually, the scheelite is fine in embedded granularity and coarse in embedded granularity, and the gangue minerals containing calcium carbonate and the like are overground by one-time complete dissociation of the target mineral, so that the floatation separation of fluorite and calcium carbonate minerals is difficult, and meanwhile, the recovery rate of tungsten is reduced in the subsequent tungsten floatation. According to the application, a segmented grinding process is adopted according to the embedding characteristics of fluorite and scheelite, a fluorite flotation section is coarsely ground, and a scheelite flotation section is finely ground, so that the beneficiation index of fluorite and scheelite is improved.
Patent No. CN102489393A discloses that scheelite bulk flotation-fluorite separation-fluorite rough concentrate regrinding and recleaning-fluorite concentrate acid leaching obtain scheelite concentrate and fluorite concentrate. The fluorite rough concentrate is regrind, the grinding fineness is 75-85 percent, the fluorite ore fine grinding of calcium carbonate-rich minerals is unfavorable for improving the concentrate grade, the fluorite concentrate grade reaches more than 97 percent, acid leaching is needed, the process flow is complex, the current environmental protection requirement is stricter, and the control on sulfuric acid and hydrochloric acid is stricter, so that the practicability of the process technology is reduced.
Patent No. CN104084315A discloses that the pH value is controlled by adding an adjusting agent and a combination inhibitor is added to the mixture of starch and water glass or acid water glassAnd (3) the mixture of CMC (CMC) carboxymethyl cellulose and water glass or acid water glass is used for preferentially floating fluorite and refloating tungsten minerals, so that the fluorite and tungsten can be efficiently recovered. The defects that fluorite is difficult to float and recycle and the beneficiation recovery rate is low due to the loss of fluorite in tungsten flotation concentrate when tungsten minerals are subjected to preferential flotation and the strong inhibition of inhibitor on fluorite during tungsten flotation are avoided; obtaining mineral separation indexes: fluorite concentrate contains CaF 2 96.41% of WO 3 0.09%, and the recovery rate of fluorite to raw ore is 74.27%; WO-containing tungsten concentrate obtained by white tungsten flotation 3 3.0% and recovery rate of 73.37%. However, the combination inhibitor has strong inhibition capability, and leads to unstable fluorite and tungsten beneficiation indexes.
Disclosure of Invention
The application aims to provide a flotation method for high-calcium type tungsten fluorite ore.
In order to achieve the above purpose, the present application provides the following technical solutions:
a flotation method of high-calcium tungsten fluorite ore, comprising the following steps:
(1) Grinding the high-calcium tungsten fluorite ore to obtain ore pulp; sequentially adding a pH regulator, a combined inhibitor 1 and a collecting agent into ore pulp for roughing, adding a capturing agent for three scavenging, and adding the combined inhibitor 1 for seven concentrating to obtain fluorite concentrate products and tailings;
(2) Concentrating tailings and then grinding to obtain ore pulp for tungsten flotation; sequentially adding an regulator, a combined inhibitor 2 and a collector into ore pulp for roughing, wherein the pH value of the ore pulp is controlled between 10 and 12; adding a capturing agent for four scavenging, and adding a combined inhibitor 2 for three concentration to obtain tungsten rough concentrate;
WO in the high calcium carbonate type tungsten fluorite ore 3 The content is 0.10 to 0.80 percent, caF 2 The content is 15-55%, caCO 3 The content is 15-40%;
the pH regulator is strong acid, the combined inhibitor 1 is a mixed reagent prepared by mixing (1-4): 1-3 by mass ratio of oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch; the collector is one or two of oleic acid, modified oleic acid, 731 or 733 oxidized paraffin soap and sodium dodecyl sulfate; the regulator is sodium carbonate and sodium hydroxide; the combined inhibitor 2 is a mixture of water glass and aluminum sulfate.
CaCO 3 Tungsten fluorite ore with 15-40% content belongs to high calcium tungsten fluorite ore. The surface chemical properties of the calcium carbonate, the scheelite and the fluorite (calcium fluoride) are similar, and the floatability is similar and difficult to separate.
During flotation, a large amount of calcium ion active sites are dissolved on the surfaces of high-content calcium carbonate minerals and scheelite minerals in the high-calcium tungsten fluorite ore, and Fe released by ferrochrome lignin in ore pulp system 2+ And Cr (V) 3+ The active component Fe for inhibiting scheelite flotation and calcite flotation is formed by absorbing calcium ions with oxalic acid, water glass and lignin sulfonic acid 2+ /Cr 3+ Oxalic acid-water glass polymer, fe 2+ /Cr 3 + -oxalic acid-lignin sulfonic acid polymer, carboxymethyl starch and Fe 3+ /Cr 3+ The surface hydrophilicity of scheelite and calcium carbonate minerals is greatly enhanced, the solubility of the scheelite and the calcium carbonate minerals is increased, and the collector is prevented from being adsorbed, so that the scheelite and the calcium carbonate minerals are separated as much as possible, and the flotation efficiency is improved.
Further, 50-70% of the particles in the pulp have a particle size of 0.074mm or less.
Further, the pH regulator is sulfuric acid, the rough concentration amount of the sulfuric acid is 0-800 g/t, and the pH is 5.5-7.0. Too low pH and too large sulfuric acid consumption can analyze the collector, so that the collector effect is poor and fluorite recovery is affected; the pH is too high, so that fluorite, calcite and scheelite are difficult to separate, and the pulp environment suitable for realizing the separation of the fluorite, the calcite and the scheelite is weak acid-neutral.
Further, the dosage of the combined inhibitor 1 in roughing is 100-250 g/t.
When the inhibitor is used excessively, fluorite minerals are inhibited, and the fluorite recovery rate is low; when the inhibitor is used too little, calcium-containing gangue minerals such as calcium carbonate float upwards, fluorite concentrate has poor quality, and tungsten is seriously lost in fluorite products.
Further, in the step (1), the addition amount of the collector in roughing is 300-800 g/t. Excessive collecting agent quantity influences the separation effect among fluorite, scheelite and calcite; the collecting agent is too small, and the recovery rate of fluorite is low.
The g/t of the application refers to the mass of the medicament added into each ton of crude ore, and the percentages are mass percentages.
Further, the addition amount of sodium carbonate in the regulator is 800-2000 g/t, and the addition amount of sodium hydroxide is 100-400 g/t. When the sodium carbonate or sodium hydroxide is excessive, the grade of the scheelite flotation rough concentrate is low; when the amount of sodium carbonate or sodium hydroxide is too small, the recovery rate of white tungsten is low.
In the combined inhibitor 2, the addition amount of water glass in roughing is 800-2000 g/t, and the addition amount of aluminum sulfate in roughing is 200-500 g/t. When the water glass or aluminum sulfate is excessive, the recovery rate of white tungsten is low; the grade of the scheelite flotation rough concentrate is low when the water glass or aluminum sulfate content is too small.
Further, in the step (2), the addition amount of the collector in roughing is 400-800 g/t. The collecting agent is excessive, and the grade of the scheelite rough concentrate is low; the collecting agent is too little, and the recovery rate of white tungsten is low.
Further, the combination inhibitor is added for the first time, the third time, the fifth time and the seventh time when the fluorite rough concentrate is selected in the step (1), and the addition amount of each time is 5-60 g/t. The water glass is added for the second time of fine selection, the fourth time of fine selection and the sixth time of fine selection, and the adding amount of each time is 100-600 g/t. Different inhibitors are added for different beneficiation operations, and the aim is to achieve staged inhibition. Because the inhibitor has strong and weak points, the sectional inhibition can effectively ensure the mineral separation indexes of tungsten and fluorite, and the condition that the mineral separation indexes of tungsten and fluorite are influenced by the excessively strong inhibition or the excessively weak inhibition cannot occur. For example, the water glass has weak inhibition capability and the combined inhibitor has strong inhibition capability, and the adoption of a sectional inhibition method is beneficial to the improvement of fluorite mineral separation indexes and the subsequent recovery of tungsten. It is also because the amount of the combined inhibitor 1 needs to be controlled with a relatively high accuracy, otherwise, the phenomenon of overdriving or not inhibiting in place easily occurs. Therefore, a staged inhibition method is adopted, and specific steps adopt inhibitors with specific strength, so that the effective separation of fluorite, calcite and scheelite is realized, the separation effect is improved to the greatest extent, and the flotation efficiency and the ore grade are improved.
Further, 50-100 g/t of collecting agent is added in each scavenging in the step (1). The collecting agent is excessive, and the fluorite concentrate grade is low; the collecting agent is too small, and the recovery rate of fluorite is low.
Further, 50-200 g/t of collecting agent is added in each scavenging in the step (2). The collecting agent is excessive, the grade of the scheelite rough concentrate is low, and the inhibitor dosage is correspondingly increased in order to ensure the grade of the concentrate, so that the beneficiation cost is increased; the collecting agent is too little, and the recovery rate of white tungsten is low.
Further, 600-2000 g/t of water glass and 100-300 g/t of aluminum sulfate are added in each carefully selecting step (2). When the water glass or aluminum sulfate is excessive, the recovery rate of white tungsten is low; the grade of the scheelite flotation rough concentrate is low when the water glass or aluminum sulfate content is too small.
Further, the modified oleic acid in the step (1) and the step (2) is prepared by mixing oleic acid and sodium carbonate according to a weight ratio of 5:1.
The modification makes oleic acid change from molecular state to ionic state, so that the solubility is better, and the flotation efficiency can be improved.
The application also claims a high calcium carbonate type tungsten fluorite ore floatation inhibitor, which is a mixed reagent prepared by mixing oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch according to the mass ratio of (1-4) (1-3). Too much or too little of any one component in the combination inhibitor can influence the inhibition effect of the combination inhibitor, when oxalic acid or ferrochrome lignin or carboxymethyl starch is too much, fluorite can be inhibited, so that the recovery rate of fluorite is low, and meanwhile, scheelite can be too strongly inhibited to be difficult to float upwards; too little oxalic acid or ferrochrome lignin or carboxymethyl starch can cause low grade of fluorite concentrate, and the loss of scheelite during fluorite flotation is large; too large a water glass ratio can affect fluorite recovery. Thus, the respective proportions of the individual components are adjusted according to the different types of ore.
The application is further explained below:
the application creatively selects to add different inhibitors in different carefully selecting operations, and aims to realize sectional inhibition, and the sectional inhibition can effectively ensure the ore dressing index of fluorite because the inhibitors have strong and weak fractions, so that the condition that the ore dressing index is influenced by the excessively strong inhibition or the excessively weak inhibition is avoided. For example, the water glass has weak inhibition capability and the combined inhibitor has strong inhibition capability, and the fluorite and tungsten ore dressing index is improved by adopting a sectional inhibition method.
The combined inhibitor is brown and white powdery solid and is easy to dissolve in water. The ferrochrome lignin is synthesized by taking sulfuric acid, ferrous sulfate, sodium dichromate and calcium lignosulfonate as raw materials. Under the condition that pH value in ore pulp is 5-6, calcium ion active sites are dissolved on the surfaces of calcium carbonate minerals and scheelite minerals, and Fe released by ferrochrome lignin in ore pulp system 2+ And Cr (V) 3+ The active component Fe for inhibiting scheelite flotation and calcite flotation is formed by absorbing calcium ions with oxalic acid, water glass and lignin sulfonic acid 2+ /Cr 3+ Oxalic acid-water glass polymer, fe 2+ /Cr 3+ -oxalic acid-lignin sulfonic acid polymer, carboxymethyl starch and Fe 3+ /Cr 3+ Strong adsorption occurs between the two, which greatly enhances the hydrophilicity of the surfaces of scheelite and calcium carbonate minerals, increases the solubility of the scheelite and calcium carbonate minerals and prevents the collector from adsorbing the scheelite and calcium carbonate minerals. And during scheelite flotation, the restrained scheelite is activated by adding the regulator, so that the scheelite is effectively recovered. The combination of the scheme of the application can inhibit the synergistic effect of the combination of different inhibitors of oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch, and a plurality of polar groups are formed on the surfaces of scheelite and calcium carbonate minerals to adsorb the scheelite and calcium carbonate minerals, so that the scheelite and the water glass are hydrophilic and inhibited, and the influence on the subsequent scheelite flotation activation recovery is small. Meanwhile, the inhibition effect of the first, third, fifth and seventh fine combinations is maximized by combining the process of the application with the sectional inhibition, and then the inhibition of calcium carbonate is properly weakened in the rest fine combinations in the steps of fine combinations, so that the separation effect of the high calcium carbonate type tungsten fluorite ore is effectively improved.
The application has the advantages that:
1. the flotation separation method of the high calcium carbonate type tungsten fluorite ore mainly solves the problem of high-efficiency comprehensive recycling of tungsten and fluorite co-associated ores in areas such as Hunan and Fujian, and has important theoretical significance and practical value for solving the problem of high-efficiency separation of tungsten and fluorite co-associated ores in China and improving the technical level and comprehensive utilization rate of the type of mineral resources;
2. according to the flotation separation method of the high calcium carbonate type tungsten fluorite ore, disclosed by the application, the synergistic effect among oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch is utilized, so that the high-efficiency separation of scheelite, fluorite and calcite and the comprehensive recovery of tungsten and fluorite to the maximum extent are realized;
3. according to the application, oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch are used as combined inhibitors to be applied to the flotation process of tungsten and fluorite co-associated ores, so that the inhibition of scheelite is enhanced, and the purpose of realizing the efficient separation of fluorite, scheelite and calcite is achieved. The combined inhibitor is small in dosage, and the method of sectional addition is beneficial to ensuring the mineral separation indexes of fluorite and tungsten, so that the problem that the grade and recovery rate of the concentrate of tungsten and fluorite cannot be simultaneously ensured when conventional inhibitors are used at present can be effectively solved.
Drawings
FIG. 1 is a process flow diagram of a flotation technique for high calcium type tungsten fluorite ore of the present application.
Detailed Description
The following examples are intended to further illustrate the application, but not limit it, and various process schemes without substantial differences from the inventive concept are within the scope of the present application. The g/t refers to the mass of the medicament added in each ton of raw ore. The percentages are mass percentages.
Example 1:
by adopting the flotation separation method of the embodiment, certain high calcium carbonate type tungsten fluorite ore (WO in raw ore) in Hunan 3 The content is 0.55%, caF 2 The content is 35.46 percent, caCO 3 The content was 23.64%) for flotation tests. The test steps are as follows:
grinding high calcium carbonate type fluorite ore until the granularity is below 0.074mm and accounts for 50%, performing fluorite preferential floatation, and performing primary roughing, three scavenging and seven concentrating to obtain fluorite concentrate, wherein the middling sequence of each operation is returned to the previous stage of operation. Adding 400g/t of sulfuric acid in fluorite roughing, 200g/t of a combined inhibitor (a mixed reagent prepared by mixing oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch according to a mass ratio of 3:3:2:2), 600g/t of oleic acid, adding and stirring for 2min each time, and floating for 4min; adding combined inhibitor for the first time, the third time, the fifth time and the seventh time when the fluorite rough concentrate is selected, wherein the adding amount of the combined inhibitor is respectively 50g/t,40g/t,30g/t,30g/t, the adding amount of water glass for the second time, the fourth time and the sixth time is 500g/t,350g/t,200g/t, each time of adding medicine and stirring for 1min, and the flotation time is 2.5min; and (3) fluorite scavenging, namely, 150g/t and 100g/t of oleic acid are sequentially added in the first scavenging and the second scavenging, and the third scavenging is not added, wherein the stirring time for each dosing is 1min, and the floatation time for each time is 2.5min.
Concentrating fluorite flotation tailings, grinding again until the granularity is below 0.074mm and accounts for 78%, performing scheelite flotation, and performing roughing four scavenging three times of concentration to obtain tungsten rough concentrate, wherein the middlings of each operation sequentially return to the previous stage of operation. Adding 1000g/t of sodium carbonate, 200g/t of sodium hydroxide, 2000g/t of sodium silicate, 400g/t of aluminum sulfate and 800g/t of 731 oxidized paraffin soap into the scheelite rougher, stirring for 2min each time, and floating for 4min; 400g/t of water glass, 100g/t of aluminum sulfate, 150g/t of water glass for the second time, 50g/t of aluminum sulfate, 150g/t of water glass for the third time and 30g/t of aluminum sulfate are added in the first time during the selection of the scheelite rough concentrate, and the adding and stirring are carried out for 1min each time, and the flotation time is 2.5min; and (3) performing white tungsten scavenging, namely sequentially adding 731 oxidized paraffin soap 200g/t and 60g/t in the first scavenging process and the second scavenging process, wherein the third scavenging process and the fourth scavenging process are not performed, the stirring time for each dosing is 1min, and the floatation time for each floatation is 2.5min.
In order to prove that the synergistic effect exists among the components of the combination inhibitor disclosed by the application, the effect of the combination inhibitor is verified, a flotation technical process flow of the high calcium carbonate type tungsten fluorite ore disclosed by the application is adopted, a comparison test is carried out on the raw ore combination inhibitor of the embodiment 1 by respectively adopting water glass, ferrochrome lignin, carboxymethyl starch (3:2:2), water glass, ferrochrome lignin (3:4), water glass, carboxymethyl starch (3:4), oxalic acid, water glass, ferrochrome lignin, carboxymethyl starch (3:3:2:2) and the combination inhibitor disclosed by the patent number CN104084315A (water glass or acid water glass is 300-1500 g/ton, and the starch consumption is 300-800 g/ton), the medicament system and the mineral separation flow are the same as those of the embodiment 1, and the test results are shown in the table 1.
TABLE 1 example 1 and comparative test results/%
As can be seen from table 1 above: the grade of fluorite concentrate products obtained by adopting the combined inhibitor disclosed by sodium silicate, ferrochrome lignin, carboxymethyl starch, sodium silicate, ferrochrome lignin, sodium silicate, carboxymethyl starch, oxalic acid, sodium silicate, ferrochrome lignin, carboxymethyl starch and patent number CN104084315A is lower than that of fluorite concentrate obtained by adopting the fluorite flotation calcium carbonate inhibitor, and WO lost in the fluorite concentrate 3 The fluorite concentrate obtained by adopting the fluorite flotation calcium carbonate inhibitor is higher than that obtained by adopting the fluorite flotation calcium carbonate inhibitor, which shows that the combination inhibitor disclosed by the application has better selective inhibition effect on scheelite and calcium carbonate.
Example 2:
by adopting the flotation separation method of the embodiment, certain high calcium carbonate type tungsten fluorite ore (WO in raw ore) in Hunan 3 The content is 0.55%, caF 2 The content is 35.46 percent, caCO 3 The content was 23.64%) for flotation tests. The test steps are as follows:
grinding high calcium carbonate type fluorite ore until the granularity is below 0.074mm and accounts for 50%, performing fluorite preferential floatation, and performing primary roughing, three scavenging and seven concentrating to obtain fluorite concentrate, wherein the middling sequence of each operation is returned to the previous stage of operation. Adding 400g/t of sulfuric acid in fluorite roughing, 200g/t of a combined inhibitor (a mixed reagent prepared by mixing oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch according to a mass ratio of 2:3:3:2), 600g/t of oleic acid, adding and stirring for 2min each time, and floating for 4min; adding a combined inhibitor for the first concentration, the third concentration, the fifth concentration and the seventh concentration when the fluorite rough concentrate is concentrated, wherein the adding amount of each time is respectively 30g/t,40g/t,30g/t,30g/t, the adding amount of water glass for the second concentration, the fourth concentration and the sixth concentration is 500g/t,350g/t,200g/t, each time is added, stirring is carried out for 1min, and the flotation time is 2.5min; and (3) fluorite scavenging, namely, 150g/t and 100g/t of oleic acid are sequentially added in the first scavenging and the second scavenging processes, and the third scavenging is not performed, wherein the stirring time for each dosing is 1min, and the floatation time for each time is 2.5min.
Concentrating fluorite flotation tailings, grinding again until the granularity is below 0.074mm and accounts for 78%, performing scheelite flotation, and performing roughing four scavenging three times of concentration to obtain tungsten rough concentrate, wherein the middlings of each operation sequentially return to the previous stage of operation. Adding 1000g/t of sodium carbonate, 200g/t of sodium hydroxide, 2000g/t of sodium silicate, 400g/t of aluminum sulfate and 800g/t of 731 oxidized paraffin soap into the scheelite rougher, stirring for 2min each time, and floating for 4min; 400g/t of water glass, 100g/t of aluminum sulfate, 150g/t of water glass for the second time, 50g/t of aluminum sulfate, 150g/t of water glass for the third time and 30g/t of aluminum sulfate are added in the first time during the selection of the scheelite rough concentrate, and the adding and stirring are carried out for 1min each time, and the flotation time is 2.5min; and (3) performing white tungsten scavenging, namely sequentially adding 731 oxidized paraffin soap 200g/t and 100g/t in the first scavenging process and the second scavenging process, and adding the oxidized paraffin soap for the third and fourth times without adding the oxidized paraffin soap, wherein the stirring time for each dosing is 1min, and the flotation time for each flotation is 2.5min.
Example 3:
the fluorite rough concentrate is carefully selected for seven times, all combined inhibitors are added, the addition amount of each time is 30g/t,100g/t,100g/t,100g/t,50/t,50g/t and 50g/t respectively, a comparison test is carried out, the rest medicament systems and the ore dressing flow are the same as those of the example 2, and the test results are shown in the table 2.
Meanwhile, all added water glass is selected seven times during the concentration of fluorite rough concentrate, the addition amount of each time is respectively 200g/t,800g/t,60g/t,600g/t,400g/t,400g/t and 200g/t, a comparison test is carried out, the rest medicament systems and the ore dressing flow are the same as those of the embodiment 2, and the test results are shown in the table 2.
TABLE 2 test results/%
As can be seen from table 2 above: after the combination inhibitor is adjusted to a proper proportion, similar beneficiation indexes can be obtained; the selection operation adopts sectional addition of the combination inhibitor, which is beneficial to improving the mineral separation index of tungsten and fluorite. When the combination inhibitor is added in each operation, the fluorite recovery rate is reduced due to the over-strong inhibition effect, and the subsequent tungsten flotation is difficult; when water glass is added in each operation of fine selection, the inhibition capability of the inhibitor is weak, the fluorite concentrate grade is low, and the loss of tungsten in the fluorite concentrate is serious. Therefore, the application adopts the steps of adding different inhibitors in sections, adding the combined inhibitor with strong inhibition capability in the operations of the selection 1, the selection 3, the selection 5 and the selection 7, and adding the inhibitor water glass with weak inhibition capability in the operations of the selection 2, the selection 4 and the selection 6, thereby being beneficial to stabilizing and improving the ore dressing indexes of tungsten and fluorite.
Example 4:
the flotation separation method of the application is adopted to treat Fujian certain high calcium carbonate tungsten fluorite ore (WO in raw ore) 3 The content is 0.22%, caF 2 The content of CaCO is 32.11 percent 3 Content 15.44%) was subjected to a flotation test. The test steps are as follows:
grinding high calcium carbonate type fluorite ore until the granularity is below 0.074mm and accounts for 55%, performing fluorite preferential floatation, and performing primary roughing, tertiary scavenging and seven times of concentration to obtain fluorite concentrate, wherein middlings of each operation are returned sequentially. Adding 200g/t of sulfuric acid into fluorite roughing, 250g/t of combined inhibitor (a mixed reagent prepared by mixing oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch according to a mass ratio of 2:4:2:2), 800g/t of oleic acid, adding medicine each time, stirring for 2min, and floating for 4min; adding a combined inhibitor for the first time of fine selection, the third time of fine selection, the fifth time of fine selection and the seventh time of fine selection, wherein the adding amount of each time is 40g/t,30g/t,20g/t,30g/t, the adding amount of water glass for the second time of fine selection, the fourth time of fine selection and the sixth time of fine selection is 400g/t,300g/t,200g/t, each time of adding medicine and stirring for 1min, and the flotation time is 2.5min; and (3) fluorite scavenging, namely, 150g/t and 100g/t of oleic acid are sequentially added in the first scavenging and the second scavenging processes, and the third scavenging is not performed, wherein the stirring time for each dosing is 1min, and the floatation time for each time is 2.5min.
Concentrating fluorite flotation tailings, grinding again until the granularity is less than 0.074mm and accounts for 83%, performing scheelite flotation, and performing roughing four scavenging three times of concentration to obtain tungsten rough concentrate, wherein middlings in each operation are returned sequentially. Adding 1000g/t of sodium carbonate, 100g/t of sodium hydroxide, 2000g/t of sodium silicate, 300g/t of aluminum sulfate, 800g/t of 731 oxidized paraffin soap and 100g/t of modified oleic acid into the white tungsten rougher, stirring for 2min each time, and floating for 4min; 800g/t of water glass, 150g/t of aluminum sulfate, 500g/t of water glass for the second time, 70g/t of aluminum sulfate, 350g/t of water glass for the third time and 50g/t of aluminum sulfate are added in the first time during the selection of the scheelite rough concentrate, and the adding and stirring are carried out for 1min each time, and the flotation time is 2.5min; the white tungsten scavenging, 80g/t of oxidized paraffin soap is added in the first scavenging, 35g/t of modified oleic acid is added in the second scavenging, 40g/t of oxidized paraffin soap is added in the second scavenging, 18g/t of modified oleic acid is added in the third and fourth scavenging, the stirring time of each adding is 1min, and the flotation time of each time is 2.5min.
To demonstrate the superiority of the beneficiation process and the combined inhibitor of the present application, comparative tests were conducted on the crude ore of example 4 (example 4), the conventional preferential float scheelite-reflaxite process (comparative example 1), the process and the combined inhibitor of patent CN104084315A (comparative example 2), and the process and the combined inhibitor of patent CN102489393A (comparative example 3).
Comparative example 1
Grinding high calcium carbonate type tungsten fluorite ore until the granularity is below 0.074mm and accounts for 75%, performing white tungsten flotation, and performing rough concentration four times and scavenging three times to obtain tungsten rough concentrate, wherein middlings in each operation are returned sequentially. Adding 2000g/t of sodium carbonate, 400g/t of sodium hydroxide, 8000g/t of sodium silicate, 200g/t of aluminum sulfate and 800g/t of 731 oxidized paraffin soap into the scheelite rougher, adding medicine each time, stirring for 2min, and floating for 4min; when the scheelite rough concentrate is selected, 2000g/t of water glass, 50g/t of aluminum sulfate, 1000g/t of water glass for the second time, 250g/t of aluminum sulfate and 600g/t of water glass for the third time are added for 1min of stirring each time, and the flotation time is 2.5min; adding 731 oxidized paraffin soap 80g/t in the first scavenging, adding 731 oxidized paraffin soap 40g/t in the second scavenging, and adding no third and fourth, wherein the stirring time for each dosing is 1min, and the floatation time for each floatation is 2.5min.
And performing fluorite flotation on the scheelite flotation tailings, and performing primary roughing, tertiary scavenging and seven times of concentration to obtain fluorite concentrate, wherein middlings in each operation are sequentially returned. Adding 600g/t of sulfuric acid, 300g/t of sodium fluoride serving as an activator, 600g/t of combined inhibitor (acid water glass and starch) and 1000g/t of oleic acid into fluorite for rough concentration, stirring for 2min each time, and carrying out flotation for 4min; adding a combined inhibitor for the first time of fine selection, the third time of fine selection, the fifth time of fine selection and the seventh time of fine selection, wherein the adding amount of each time is 300g/t,200g/t,100g/t,100g/t, the adding amount of water glass for the second time of fine selection, the fourth time of fine selection and the sixth time of fine selection, the adding amount of each time is 400g/t,300g/t,200g/t, each time of adding medicine and stirring for 1min, and the flotation time is 2.5min; and (3) fluorite scavenging, wherein 200g/t and 100g/t of oleic acid are sequentially added in the first scavenging and the second scavenging processes, the third scavenging is not added, the stirring time of each dosing is 1min, and the flotation time of each time is 2.5min.
Comparative example 2
After grinding the high calcium carbonate type tungsten fluorite ore to a granularity below 0.074mm and accounting for 75%, the test is carried out by adopting a technological process and a combined inhibitor disclosed in patent No. CN 104084315A.
Comparative example 3
After grinding the high calcium carbonate type tungsten fluorite ore to a granularity below 0.074mm and accounting for 75%, the test is carried out by adopting a technological process and a combined inhibitor disclosed in patent No. CN 102489393A. In the test, fluorite concentrate is not subjected to acid leaching, and scheelite rough concentrate obtained after separation is not subjected to heating concentration. The test results are shown in Table 2.
TABLE 3 example 4 and comparative test results/%
As can be seen from table 4 above: the ore dressing indexes obtained by adopting the traditional preferential scheelite-refloating process (comparative example 1), the process flow and the combined inhibitor (comparative example 2) disclosed by patent number CN104084315A, the process flow and the combined inhibitor (comparative example 3) disclosed by patent number CN102489393A are poorer than the ore dressing indexes obtained by adopting the combined inhibitor and the process flow, the grade of the fluorite concentrate obtained by adopting the ore dressing indexes is lower, and the standard of high-grade fluorite cannot be reached. And after the fluorite grade is over 95%, the recovery rate needs to be increased by at least 3-5% every 1% of fluorite grade in the prior art. Therefore, the higher the grade, the lower the recovery, and the balance between the two is difficult to reach. And the comparative example adopts a large amount of inhibitor, which proves that the combined inhibitor and the process flow disclosed by the application have more advantages.
The application creatively combines oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch together, and the carboxymethyl starch contains high electronegativity carboxylic acid groups which are stronger hydrophilic groups and have good inhibiting effect on calcium-containing minerals. In addition, sulfonate and hydroxyl in the ferrochrome lignin can be combined with calcium ions to inhibit calcium carbonate minerals and scheelite; the addition of oxalic acid enhances the inhibition of scheelite, and greatly reduces the loss of scheelite in fluorite concentrate. Oxalic acid, ferrochrome lignin and carboxymethyl starch are combined with water glass to generate synergistic effect, so that the inhibition capability and selectivity of the inhibitor are more obvious compared with the improvement effect of the common inhibitor when the concentration of calcium carbonate is higher, and the subsequent activation and recovery of tungsten are facilitated. Meanwhile, the inhibition effect of the first concentration, the third concentration, the fifth concentration and the seventh concentration is maximized by combining the process of the segmented inhibition of the application, and then the inhibition of calcium carbonate and tungsten is properly weakened in the rest concentration steps, and the separation effect of the high calcium carbonate type tungsten fluorite ore is effectively improved by combining the process of the segmented inhibition with the inhibitor.
Claims (7)
1. The high-calcium tungsten fluorite flotation method is characterized by comprising the following steps of:
(1) Grinding the high-calcium tungsten fluorite ore to obtain ore pulp; sequentially adding a pH regulator, a combined inhibitor 1 and a collecting agent into ore pulp for roughing, adding a capturing agent for three scavenging, and adding the combined inhibitor 1 for seven concentrating to obtain fluorite concentrate products and tailings;
(2) Concentrating tailings and then grinding to obtain ore pulp for tungsten flotation; sequentially adding an regulator, a combined inhibitor 2 and a collector into ore pulp for roughing, wherein the pH value of the ore pulp is controlled to be 10-12; adding a capturing agent for four scavenging, and adding a combined inhibitor 2 for three concentration to obtain tungsten rough concentrate; WO in the high calcium carbonate type tungsten fluorite ore 3 The content is 0.10-0.80%, caF 2 15-55% CaCO 3 The content is 15-40%; the pH regulator is strong acid, the combined inhibitor 1 is oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch according to the mass ratio of (1-4): (1-4): (1-3): (1-3) mixing the obtained mixed reagent; the collector is one or two of oleic acid, modified oleic acid, 731 or 733 oxidized paraffin soap and sodium dodecyl sulfate; the regulator is sodium carbonate and sodium hydroxide; the combined inhibitor 2 is a mixture of sodium silicate and aluminum sulfate;
the method comprises the steps of (1) adding a combined inhibitor 1 for the first concentration, the third concentration, the fifth concentration and the seventh concentration in the concentration of fluorite rough concentrate, wherein the addition amount of each time is 5-60 g/t; adding water glass for the second selection, the fourth selection and the sixth selection, wherein the adding amount of each time is 100-600 g/t;
in the step (1), the pH regulator is sulfuric acid, the roughing dosage of the sulfuric acid is 0-800 g/t, and the pH is 5.5-7.0.
2. The method for high calcium type tungsten fluorite flotation according to claim 1, wherein the amount of the combined suppressant 1 used in roughing is 100-250 g/t.
3. The method for floating high-calcium tungsten fluorite according to claim 1, wherein in the step (1), the addition amount of the collector in roughing is 300-800 g/t; the addition amount is 50-200 g/t during scavenging; in the step (2), the addition amount of the collector in roughing is 400-800 g/t; the addition amount is 50-200 g/t during scavenging.
4. The method for floating high-calcium tungsten fluorite according to claim 1, wherein the addition amount of sodium carbonate in the regulator is 800-2000 g/t and the addition amount of sodium hydroxide is 100-400 g/t.
5. The method for flotation of high calcium type tungsten fluorite according to claim 1, wherein in the combined inhibitor 2, the addition amount of water glass in roughing is 800-2000 g/t, and the addition amount of aluminum sulfate in roughing is 200-500 g/t.
6. The method of claim 1, wherein the collector is one or both of 731 or 733 oxidized paraffin soap, oleic acid, or modified oleic acid.
7. The flotation inhibitor for the high-calcium tungsten fluorite is characterized by comprising oxalic acid, water glass, ferrochrome lignin and carboxymethyl starch according to the mass ratio of (1-4): (1-4): (1-3): (1-3) mixing the obtained mixed reagent.
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