CN113369005A - Beneficiation method for mixed type refractory tungsten ore - Google Patents
Beneficiation method for mixed type refractory tungsten ore Download PDFInfo
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- CN113369005A CN113369005A CN202110520193.3A CN202110520193A CN113369005A CN 113369005 A CN113369005 A CN 113369005A CN 202110520193 A CN202110520193 A CN 202110520193A CN 113369005 A CN113369005 A CN 113369005A
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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
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
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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
- B03D1/004—Organic compounds
- B03D1/01—Organic compounds containing nitrogen
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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
- 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
- B03D2203/04—Non-sulfide ores
Abstract
The invention relates to a beneficiation method of mixed type refractory tungsten ore, which comprises the following steps: the method comprises the steps of grinding crushed raw black and white tungsten paragenetic ore to obtain ore pulp; the pH value of the ore pulp is 7.0-9.0, and an inhibitor, an activating agent lead nitrate and a collecting agent are added to perform mixed tungsten roughing to obtain tungsten rough concentrate ore pulp and rough tailings ore pulp respectively; thirdly, performing two times of mixed tungsten scavenging on the rough tailings slurry to obtain tungsten scavenging tailings I; fourthly, performing weak magnetic deironing operation on the tungsten rough concentrate ore pulp to respectively obtain a magnetic iron product and magnetic separation tailing ore pulp; fifthly, performing strong magnetic rough concentration and scavenging on the magnetic separation tailing slurry to obtain a wolframite concentrate product and scavenging operation tailings respectively; sixthly, performing dense dehydration on the scavenged operation tailings to obtain ore pulp with the concentration of 60-70%; and carrying out flotation operation on 60-70% of ore pulp to obtain scheelite concentrate and tungsten scavenging tailings II respectively. The invention effectively realizes the effective separation and enrichment of the wolframite and the scheelite.
Description
Technical Field
The invention relates to the technical field of non-ferrous metal beneficiation, in particular to a beneficiation method of mixed type refractory tungsten ore.
Background
Tungsten is one of the irreplaceable basic materials of national economy and modern national defense, is an important strategic material, is widely applied to important fields of aerospace, mechanical manufacturing, national defense industry and the like, and therefore the nation pays high attention to the development and utilization of tungsten resources.
At present, methods for successfully recovering scheelite and wolframite by flotation from complex polymetallic ores containing sulfide ore, scheelite, wolframite, cassiterite, garnet, fluorite, calcite and the like include the GY method, the CY method and the persimmon bamboo garden method (a combination of the GY method and the CY method). The method is characterized in that a chelating collecting agent (benzohydroxamic acid or nitrosophenylhydroxylamine ammonium salt) is adopted to perform mixed flotation on the black and white tungsten in neutral ore pulp to obtain black and white tungsten mixed flotation rough concentrate containing 5-40% of tungsten trioxide, and the tungsten recovery rate is 75-80%. The methods make great progress in mineral separation of black and white tungsten paragenic ores. Although the heating stirring flotation has good effect on the scheelite concentration in the rough concentrate, a large amount of water glass, sodium sulfide and the like are added in the heating stirring flotation scheelite concentration process, so that the wolframite is strongly inhibited, great difficulty is brought to the recovery of the wolframite, and the wolframite is strongly inhibited and difficult to activate, so that the scheelite concentration recovery rate and the wolframite concentrate grade are both low and unstable.
The wolframite intergrowth belongs to refractory ores, wherein calcium-rich fluorite, calcite and calcium-and magnesium-rich tremolite are often associated, the surface properties of the gangue and the scheelite are similar, and a large amount of inhibitor is often required to be added for inhibiting the gangue. Common inhibitors include water glass, sodium hexametaphosphate, sodium fluorosilicate, carboxymethyl cellulose and the like. In the mixing and floating of the scheelite and wolframite paragenetic ore, the lead nitrate is added, which is beneficial to enhancing the collecting capability of the chelating agent on the scheelite and reducing the using amount of the collecting agent. The collector adopted by the mixed flotation of the black-white tungsten paragenic ore is generally a combined collector used by combining a fatty acid collector, a chelating collector and the fatty acid collector. In the aspect of the process flow, the selection of a proper process flow is also important, and the selection of the proper process flow is also the key for obtaining a better mineral separation technical index.
Disclosure of Invention
The invention aims to solve the technical problem of providing a beneficiation method of mixed type refractory tungsten ore for realizing effective separation and enrichment of scheelite and wolframite.
In order to solve the problems, the beneficiation method of the mixed type refractory tungsten ore comprises the following steps:
firstly, grinding ore:
grinding the crushed black-white tungsten paragenetic ore raw ore to obtain ore pulp;
mixing tungsten for roughing:
adding 1000-1500 g/t of sodium carbonate into the ore pulp according to the dry weight of the crushed raw ore of the black-white tungsten paragenic ore until the pH value of the ore pulp is 7.0-9.0, and then adding 800-1200 g/t of an inhibitor, 500-600 g/t of an activating agent lead nitrate and 400-600 g/t of a collecting agent for mixed tungsten roughing to respectively obtain tungsten rough concentrate ore pulp and rough tailings ore pulp;
thirdly, scavenging with mixed tungsten:
performing two times of mixed tungsten scavenging operation on the rougher tailing pulp to obtain tungsten scavenging tailings I;
four weak magnetic iron removal operations:
carrying out magnetic separation on the tungsten rough concentrate ore pulp by adopting a permanent magnet drum type low intensity magnetic separator under the condition that the magnetic field intensity is 0.2T to respectively obtain a magnetic iron product and magnetic separation tailing ore pulp;
fifthly, performing strong magnetic separation on tungsten:
performing strong magnetic rough separation on the magnetic separation tailing pulp by adopting a high-gradient magnetic separator under the condition that the magnetic field intensity is 1.0-1.5T to respectively obtain black tungsten concentrate and strong magnetic separation tailing pulp; carrying out strong magnetic scavenging on the strong magnetic separation tailing pulp under the condition that the magnetic field intensity is 0.6-0.8T to respectively obtain magnetic separation middlings and scavenging operation tailings; the magnetic separation middling and the black tungsten concentrate are combined into a black tungsten concentrate product;
sixthly, performing dense dehydration:
concentrating and dehydrating the scavenging operation tailings to respectively obtain ore pulp and overflow water with the concentration of 60-70%;
scheelite flotation operation:
and performing scheelite roughing operation, scheelite scavenging operation and scheelite concentration operation on the ore pulp with the concentration of 60-70% to respectively obtain scheelite concentrate and tungsten scavenging tailings II.
The conditions for grinding the ores in the step mean that the mass ratio of the crushed raw ores of the black-white tungsten paragenetic ores to water is 1: 1; according to the dry weight of the black and white tungsten paragenetic raw ore, the grinding fineness of the ground ore product is-74 mu m and accounts for 75-80%.
The step three, twice mixed tungsten scavenging operation refers to adding 100-200 g/t of inhibitor and 80-120 g/t of collector into the rough concentration tailing pulp to perform once tungsten scavenging operation according to the dry ore weight of the crushed black-white tungsten paragenic ore raw ore, so as to obtain once scavenged tailing pulp and once scavenged middling respectively, and the once scavenged middling enters the mixed tungsten rough concentration; adding 50-80 g/t of inhibitor and 30-50 g/t of collecting agent into the primary scavenging tailing pulp to carry out secondary tungsten scavenging to respectively obtain the tungsten scavenging tailings I and secondary scavenging middlings, and returning the secondary scavenging middlings to the primary tungsten scavenging operation.
The inhibitor is prepared by mixing water glass, sodium polyacrylate, sodium sulfite and sodium hexametaphosphate in a ratio of 2-4: 1: 1: 1, in a mass ratio of 1.
The collecting agent is prepared by mixing hydroximic acids, fatty acids and glycerol monostearate according to the weight ratio of 1-2: 0.5-1.0: 0.3, and heating and stirring in a water bath for 0.5 to 1.0 hour under the conditions that the temperature is 30 to 50 ℃ and the stirring speed is 600 to 900 r/min.
The hydroxamic acid is one or more of octyl hydroxamic acid, salicylhydroxamic acid and benzohydroxamic acid.
The fatty acid is one or more of oleic acid, oxidized paraffin soap, sodium oleate and tall soap.
The scheelite roughing operation in the step S-S is that 1500-2000 g/t of water glass and 733300-500 g/t of oxidized paraffin soap are added into ore pulp with the concentration of 60-70% according to the dry weight of the crushed raw ore of the black-white tungsten paragenic ore, then the ore pulp is heated to 85-95 ℃ and stirred for 60 minutes, and the scheelite rough concentrate ore pulp and the scheelite roughing tailing ore pulp are respectively obtained.
The scheelite scavenging operation in the step-wise includes that collecting agent oxidized paraffin soap 73360-100 g/t is added into scheelite roughing tailing pulp to perform primary scavenging operation according to the dry weight of the crushed raw ore of the wolframite and wolframite, so that primary scheelite scavenging tailing pulp and primary scheelite scavenging middling are obtained respectively, and the primary scheelite scavenging middling enters the scheelite roughing operation; adding a collecting agent oxidized paraffin soap 73330-50 g/t into the primary scheelite scavenging tailing pulp to carry out secondary scavenging to obtain the tungsten scavenging tailing II and secondary scheelite scavenging middlings respectively, and returning the secondary scheelite scavenging middlings to the primary scavenging operation.
The scheelite concentration operation in step-nickle is to perform concentration operation on scheelite rough concentrate pulp for four times according to a conventional method without adding any medicament to obtain scheelite concentrate; and the middlings in the first concentration enter the scheelite roughing operation, and the middlings in the second to fourth concentrations return to the previous operation cycle in sequence.
Compared with the prior art, the invention has the following advantages:
1. in the invention, a magnetic separation-flotation combined principle process flow is adopted, and after regulating agent sodium carbonate, inhibitor, activating agent lead nitrate and collecting agent are added in tungsten ore mixed flotation operation, the tungsten ore mixed rough concentrate is obtained by primary rough concentration; performing weak magnetic iron removal on the tungsten mixed rough concentrate, and performing strong magnetic tungsten separation on tailings subjected to weak magnetic iron removal to obtain black tungsten concentrate; the tailings after the strong magnetic tungsten separation operation are subjected to dense dehydration, and the scheelite high-temperature flotation operation is performed after the conventional agent is added, so that the scheelite and the wolframite are effectively separated and enriched.
2. The inhibitor is prepared by mixing water glass, sodium polyacrylate, sodium sulfite and sodium hexametaphosphate, wherein: the water glass is an inorganic colloid and has a good inhibition effect on gangue minerals such as quartz and silicate. The main component for inhibiting in the water glass solution is H2SiO3、HSiO3-The two substances can be adsorbed on the surface of the mineral and have strong hydrophilicity, so that the mineral can be hydrophilic to play an inhibiting role after being adsorbed on the surface of the mineral, and when the two substances are combined with sodium hexametaphosphate for use, the selective inhibiting effect of water glass can be enhanced; the sodium polyacrylate is a macromolecular organic matter with the molecular weight of 800-1000 ten thousand, has better selective inhibition performance, is an inhibitor containing calcium gangue minerals, and is dissolved in water to generate-COO-Selectively reacting with calcium-containing gangue minerals to generate hydrophilic-COOCa on the surface of the gangue minerals, so that the calcium-containing gangue minerals are hydrophilic and inhibited, and the effect of effectively separating useful minerals from gangue is achieved; the sodium hydrosulfite has an inhibiting effect on pyrite, chalcopyrite and the like under the condition of low alkalinity; sodium hexametaphosphate is an inhibitor for carbonates such as limestone and calcite and silicates and quartz, and is generally considered to be partially ionized into anions in an aqueous solution, and the anions form insoluble salts with calcium ions on the surface of minerals and are converted into stable soluble complexes to achieve an inhibiting effect.
3. The collecting agent is prepared by mixing hydroximic acids, fatty acids and glycerol monostearate in proportion, and heating and stirring in a water bath for 0.5-1.0 hour at the temperature of 30-50 ℃ and the stirring speed of 600-900 r/min; the composite collector has the characteristics of strong collecting capability of the fatty acid collecting agent and strong selectivity of the chelating collecting agent, can exert the positive synergistic effect of the two types of collecting agents, and effectively improves the selective collecting capability of the collecting agent on the mixed tungsten ore by adding the emulsifier.
The novel chelating hydroximic acid is a novel chelating collecting agent. In the weakly alkaline ore pulp, hydroximic acid ions are chelated on the surface of scheelite, a multi-molecular adsorption layer is formed on the surface of the scheelite, the nonpolar part of the molecules can be adsorbed on the original monomolecular layer in a hydrogen bond form, and the activity of the ion-molecule co-adsorption is increased, so that the adsorption capacity of the scheelite is greatly enhanced; meanwhile, the collector is also an effective collector for fine-grained wolframite.
The fatty acid collector has strong collecting capacity on the wolframite, and a flotation mechanism of the fatty acid collector shows that Mn particles on the surface of the wolframite are active particles reacted with sodium oleate, and the sodium oleate is chemically adsorbed on the surface of the wolframite to generate oleate so as to achieve the effect of collecting the wolframite.
The glycerol monostearate is a good emulsifier, the addition of the glycerol monostearate increases the emulsifying dispersibility of the collecting agent in ore pulp, so that the performance of the emulsified collecting agent is more stable, the dispersibility of the collecting agent in the ore pulp is better, and the collecting capability of the collecting agent can be greatly improved.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a flow chart of the present invention.
Detailed Description
As shown in fig. 1, a mixed type refractory tungsten ore beneficiation method includes the following steps:
firstly, grinding ore:
grinding the crushed black-white tungsten paragenetic ore raw ore to obtain ore pulp of basic mineral effective monomer dissociation.
The ore grinding conditions mean that the mass ratio of the crushed black-white tungsten paragenetic ore raw ore to the water is 1: 1; according to the dry weight of the black and white tungsten paragenetic raw ore, the grinding fineness of the ground ore product is-74 mu m and accounts for 75-80%.
Mixing tungsten for roughing:
adding 1000-1500 g/t of sodium carbonate (a) into ore pulp according to the dry weight of the crushed black-white tungsten paragenic ore raw ore until the pH value of the ore pulp is 7.0-9.0, and then adding 800-1200 g/t of inhibitor (b), 500-600 g/t of activating agent lead nitrate (c) and 400-600 g/t of collecting agent (d) for mixed tungsten roughing to respectively obtain tungsten rough concentrate ore pulp and rougher tailing ore pulp.
Wherein: the inhibitor is prepared by mixing water glass, sodium polyacrylate, sodium sulfite and sodium hexametaphosphate in a ratio of 2-4: 1: 1: 1, in a mass ratio of 1.
The collecting agent is prepared by mixing hydroximic acids, fatty acids and glycerol monostearate according to the weight ratio of 1-2: 0.5-1.0: 0.3, and heating and stirring in a water bath for 0.5 to 1.0 hour under the conditions that the temperature is 30 to 50 ℃ and the stirring speed is 600 to 900 r/min. The hydroxamic acid is one or more of octyl hydroxamic acid, salicylhydroxamic acid and benzohydroxamic acid. The fatty acid is one or more of oleic acid, oxidized paraffin soap, sodium oleate and tall soap.
Thirdly, scavenging with mixed tungsten:
and carrying out two times of mixed tungsten scavenging operation on the rougher tailing pulp to obtain tungsten scavenging tailings I. The specific process is as follows:
adding 100-200 g/t of inhibitor (b) and 80-120 g/t of collecting agent (d) into the rough concentration tailing pulp according to the dry weight of the crushed black and white tungsten paragenic raw ore to perform a primary tungsten scavenging operation to respectively obtain primary scavenging tailing pulp and primary scavenging middlings, and enabling the primary scavenging middlings to enter mixed tungsten rough concentration; adding 50-80 g/t of inhibitor (b) and 30-50 g/t of collector (d) into the primary scavenging tailing slurry to perform secondary tungsten scavenging to obtain tungsten scavenging tailings I and secondary scavenging middlings respectively, and returning the secondary scavenging middlings to primary tungsten scavenging operation.
Wherein: the inhibitor and the collector are synchronously processed.
Four weak magnetic iron removal operations:
and (3) carrying out magnetic separation on the tungsten rough concentrate ore pulp by adopting a permanent magnet drum type low intensity magnetic separator under the condition that the magnetic field intensity is 0.2T to respectively obtain a magnetic iron product and magnetic separation tailing ore pulp.
Fifthly, performing strong magnetic separation on tungsten:
performing strong magnetic rough separation on the magnetic separation tailing pulp by adopting a high-gradient magnetic separator under the condition that the magnetic field intensity is 1.0-1.5T to respectively obtain black tungsten concentrate and strong magnetic separation tailing pulp; carrying out strong magnetic scavenging on the strong magnetic separation tailing pulp under the condition that the magnetic field intensity is 0.6-0.8T to respectively obtain magnetic separation middlings and scavenging operation tailings; and combining the magnetic separation middling and the black tungsten concentrate into a black tungsten concentrate product.
Sixthly, performing dense dehydration:
concentrating and dehydrating the scavenging operation tailings, concentrating and filtering water and a flotation agent to obtain ore pulp and overflow water with the concentration of 60-70% respectively.
Scheelite flotation operation:
and (3) performing scheelite roughing operation, scheelite scavenging operation and scheelite concentration operation on the ore pulp with the concentration of 60-70% to respectively obtain scheelite concentrate and tungsten scavenging tailings II. The specific process is as follows:
the scheelite roughing operation is that according to the dry weight of the crushed raw scheelite and black and white tungsten paragenetic ore, 1500-2000 g/t of water glass (e) and 300-500 g/t of oxidized paraffin soap 733 (f) are added into ore pulp with the concentration of 60% -70%, then the ore pulp is heated to 85-95 ℃ and stirred for 60 minutes, and scheelite rough concentrate ore pulp and scheelite roughing tailing ore pulp are respectively obtained.
The scheelite scavenging operation is to add 60-100 g/t of collecting agent oxidized paraffin soap 733 (f) into scheelite roughing tailing pulp to perform primary scavenging operation according to the dry weight of the crushed raw ore of the wolframite and scheelite, so as to respectively obtain primary scheelite scavenging tailing pulp and primary scheelite scavenging middling, and the primary scheelite scavenging middling enters the scheelite roughing operation; adding 30-50 g/t of collecting agent oxidized paraffin soap 733 (f) into the primary scheelite scavenging tailing pulp to carry out secondary scavenging to respectively obtain tungsten scavenging tailings II and secondary scheelite scavenging middlings, and returning the secondary scheelite scavenging middlings to the primary scavenging operation.
The scheelite concentration operation means that scheelite rough concentrate pulp is subjected to concentration operation for four times according to a conventional method without adding any medicament to obtain scheelite concentrate; wherein, the first-time concentration middlings enter scheelite roughing operation, and the second-fourth-time concentration middlings return to the previous operation cycle in sequence.
Example 1:
the raw ore of the mixed type wolframite ore contains about 1.05 percent of WO3, and the proportion of the wolframite ore is 2: 4.5. The main metal minerals in the ore are wolframite and scheelite, and then wolframite, magnetite, pyrrhotite, pyrite and a small amount of molybdenite, and the gangue minerals mainly comprise quartz, and then fluorite, mica, plagioclase, chlorite, a small amount of wollastonite, apatite and the like. The tungsten mineral in the ore exists mainly in the form of wolframite and scheelite. The usable wolframite and scheelite in the ore has uneven granularity, close embedding relation with gangue, more dispersed distribution and complex embedding state, and belongs to ore which is difficult to select. The test results are shown in Table 1.
The specific process is as follows:
firstly, grinding ore:
mixing the crushed black-white tungsten paragenetic ore raw ore and water according to the proportion of 1: 1, grinding the raw ore by a ball mill, wherein the grinding fineness of the ground product is-74 mu m accounting for 80 percent of the dry weight of the raw ore of the black-white tungsten paragenic ore in an ore grinding machine, and obtaining the ore pulp of the dissociation of the basic mineral effective monomers.
Mixing tungsten for roughing:
adding 1000g/t of sodium carbonate (a) into ore pulp according to the dry weight of the crushed black-white tungsten paragenic ore raw ore until the pH value of the ore pulp is 7.0, and then adding 800 g/t of inhibitor (b), 600g/t of activating agent lead nitrate (c) and 600g/t of collecting agent (d) for mixed tungsten roughing to respectively obtain tungsten rough concentrate ore pulp and rougher tailing ore pulp.
Wherein: the inhibitor is prepared by mixing water glass, sodium polyacrylate, sodium sulfite and sodium hexametaphosphate in a ratio of 2: 1: 1: 1, in a mass ratio of 1.
The collecting agent is prepared by mixing benzohydroxamic acid, oxidized paraffin soap and glycerol monostearate according to the proportion of 1: 0.5: 0.3, and heating and stirring in a water bath for 0.5 to 1.0 hour under the conditions that the temperature is 30 to 50 ℃ and the stirring speed is 600 to 900 r/min.
Thirdly, scavenging with mixed tungsten:
adding 100g/t of inhibitor (b) and 120g/t of collecting agent (d) into the rough concentration tailing pulp according to the dry ore weight of the crushed black-white tungsten paragenic ore raw ore to carry out a tungsten scavenging operation to respectively obtain a primary scavenging tailing pulp and a primary scavenging middling, and feeding the primary scavenging middling into mixed tungsten roughing; adding 50g/t of inhibitor (b) and 50g/t of collecting agent (d) into the primary scavenging tailing pulp to carry out secondary tungsten scavenging to respectively obtain tungsten scavenging tailings I and secondary scavenging middlings, and returning the secondary scavenging middlings to primary tungsten scavenging operation.
Wherein: the inhibitor and the collector are synchronously processed.
Four weak magnetic iron removal operations:
and (3) carrying out magnetic separation on the tungsten rough concentrate ore pulp by adopting a permanent magnet drum type low intensity magnetic separator under the condition that the magnetic field intensity is 0.2T to respectively obtain a magnetic iron product and magnetic separation tailing ore pulp.
Fifthly, performing strong magnetic separation on tungsten:
performing strong magnetic roughing on the magnetic separation tailing pulp by adopting a high-gradient magnetic separator under the condition that the magnetic field intensity is 1.5T to respectively obtain wolframite concentrate and strong magnetic separation tailing pulp; carrying out strong magnetic scavenging on the strong magnetic tailing pulp under the condition that the magnetic field intensity is 0.8T to respectively obtain magnetic separation middlings and scavenging operation tailings; and combining the magnetic separation middling and the black tungsten concentrate into a black tungsten concentrate product.
Sixthly, performing dense dehydration:
concentrating and dehydrating the scavenging operation tailings, concentrating and filtering water and a flotation agent to respectively obtain ore pulp with the concentration of 60% and overflow water.
Scheelite flotation operation:
the scheelite roughing operation is that 2000g/t of water glass (e) and 300g/t of oxidized paraffin soap (f) are added into ore pulp with the concentration of 60 percent according to the dry weight of the crushed raw ore of the black and white tungsten paragenic ore, and then the ore pulp is heated to 85-95 ℃ and stirred for 60 minutes to respectively obtain scheelite rough concentrate ore pulp and scheelite roughing tailing ore pulp.
The scheelite scavenging operation is to add 60g/t of collecting agent oxidized paraffin soap 733 (f) into scheelite roughing tailing pulp to perform primary scavenging operation according to the dry weight of the crushed raw ore of the wolframite and scheelite, so as to respectively obtain primary scheelite scavenging tailing pulp and primary scheelite scavenging middling, and the primary scheelite scavenging middling enters the scheelite roughing operation; adding 30g/t of collecting agent oxidized paraffin soap 733 (f) into the ore pulp of the primary scheelite scavenging tailings for secondary scavenging to respectively obtain tungsten scavenging tailings II and secondary scheelite scavenging middlings, and returning the secondary scheelite scavenging middlings to the primary scavenging operation.
The scheelite concentration operation means that scheelite rough concentrate pulp is subjected to concentration operation for four times according to a conventional method without adding any medicament to obtain scheelite concentrate; wherein, the first-time concentration middlings enter scheelite roughing operation, and the second-fourth-time concentration middlings return to the previous operation cycle in sequence.
Example 2:
a refractory mixed type black and white tungsten ore in Xinjiang, the raw ore contains WO3About 0.55 percent, and the proportion of the wolframite to the wolframite is 1: 4.2. The main metal minerals in the ore are wolframite and scheelite, and then are wolframite, magnetite, pyrrhotite, chalcopyrite, specularite, pyrite, molybdenite, a small amount of cassiterite and ilmenite, and the gangue minerals mainly comprise quartz and fluorite, and then are biotite, muscovite, plagioclase, kaolinite, chlorite, a small amount of clinoptilolite, pyrophyllite and the like. The test results are shown in Table 1.
The specific process is as follows:
firstly, grinding ore:
mixing the crushed black-white tungsten paragenetic ore raw ore and water according to the proportion of 1: 1, grinding the raw ore by a ball mill, wherein the grinding fineness of the ground product is-74 mu m and accounts for 75 percent of the dry weight of the raw ore of the black-white tungsten paragenic ore in an ore grinding machine, and obtaining the ore pulp of the dissociation of the basic mineral effective monomers.
Mixing tungsten for roughing:
according to the dry weight of the crushed black-white tungsten paragenic ore, adding 1500g/t of sodium carbonate (a) into ore pulp until the pH value of the ore pulp is 9.0, and then adding 800 g/t of inhibitor (b), 500g/t of activating agent lead nitrate (c) and 1200g/t of collecting agent (d) to carry out mixed tungsten roughing to respectively obtain tungsten rough concentrate ore pulp and rougher tailing ore pulp.
Wherein: the inhibitor is prepared by mixing water glass, sodium polyacrylate, sodium sulfite and sodium hexametaphosphate in a ratio of 4: 1: 1: 1, in a mass ratio of 1.
The collecting agent is prepared by mixing benzohydroxamic acid, oxidized paraffin soap and glycerol monostearate according to the proportion of 2: 1: 0.3, and heating and stirring in a water bath for 0.5 to 1.0 hour under the conditions that the temperature is 30 to 50 ℃ and the stirring speed is 600 to 900 r/min.
Thirdly, scavenging with mixed tungsten:
adding 200g/t of inhibitor (b) and 80g/t of collecting agent (d) into the rough concentration tailing pulp according to the dry ore weight of the crushed black-white tungsten paragenic ore raw ore to carry out a tungsten scavenging operation, respectively obtaining primary scavenging tailing pulp and primary scavenging middlings, and enabling the primary scavenging middlings to enter mixed tungsten roughing; adding 80g/t of inhibitor (b) and 30g/t of collector (d) into the primary scavenging tailing pulp to carry out secondary tungsten scavenging to respectively obtain tungsten scavenging tailings I and secondary scavenging middlings, and returning the secondary scavenging middlings to primary tungsten scavenging operation.
Wherein: the inhibitor and the collector are synchronously processed.
The weak magnetic iron removal operation is the same as that of example 1.
Fifthly, performing strong magnetic separation on tungsten:
performing strong magnetic roughing on the magnetic separation tailing pulp by adopting a high-gradient magnetic separator under the condition that the magnetic field intensity is 1.0T to respectively obtain wolframite concentrate and strong magnetic separation tailing pulp; carrying out strong magnetic scavenging on the strong magnetic tailing pulp under the condition that the magnetic field intensity is 0.6T to respectively obtain magnetic separation middlings and scavenging operation tailings; and combining the magnetic separation middling and the black tungsten concentrate into a black tungsten concentrate product.
Sixthly, performing dense dehydration:
concentrating and dehydrating the scavenging operation tailings, concentrating and filtering water and a flotation agent to respectively obtain ore pulp and overflow water with the concentration of 70%.
Scheelite flotation operation:
the scheelite roughing operation is that 1500g/t of water glass (e) and 500g/t of oxidized paraffin soap 733 (f) are added into ore pulp with the concentration of 70 percent according to the dry weight of the crushed raw ore of the black and white tungsten paragenic ore, and then the ore pulp is heated to 85-95 ℃ and stirred for 60 minutes to respectively obtain scheelite rough concentrate ore pulp and scheelite roughing tailing ore pulp.
The scheelite scavenging operation is to add 100g/t of collecting agent oxidized paraffin soap 733 (f) into scheelite roughing tailing pulp to perform primary scavenging operation according to the dry weight of the crushed raw ore of the wolframite and scheelite, so as to respectively obtain primary scheelite scavenging tailing pulp and primary scheelite scavenging middling, and the primary scheelite scavenging middling enters the scheelite roughing operation; adding a collecting agent oxidized paraffin soap 733 (f) 50g/t into the ore pulp of the primary scheelite scavenging tailings for secondary scavenging to respectively obtain tungsten scavenging tailings II and secondary scheelite scavenging middlings, and returning the secondary scheelite scavenging middlings to the primary scavenging operation.
The scheelite concentration was performed in the same manner as in example 1.
TABLE 1 technical indexes for mineral separation of the invention
As can be seen from table 1, both example 1 and example 2 obtained better beneficiation technical indexes by using the beneficiation method of the present invention.
Example 1: the grade of the wolframite concentrate reaches 45.98 percent, and the recovery rate is 24.86 percent; the grade of the scheelite concentrate reaches 63.15 percent, and the recovery rate is 54.51 percent; the comprehensive recovery rate of the wolframite is 79.37%.
Example 2: the grade of the wolframite concentrate reaches 40.15 percent, and the recovery rate is 15.40 percent; the grade of the scheelite concentrate reaches 60.03 percent, and the recovery rate is 61.41 percent; the comprehensive recovery rate of the wolframite is 76.81 percent.
Comparative example 1
The mixed tungsten ore of the same grade in the example 1 is subjected to tungsten roughing operation, the inhibitor of the tungsten roughing operation is compared with the inhibitor in the example 1 by using water glass which is a conventional chemical agent, and other chemical agent conditions are shown in the example 1. The comparative results of the mixed tungsten ore in the inhibitor test of tungsten roughing operation are shown in table 2.
Comparative example 2
The mixed tungsten ore of the same grade in the example 1 is subjected to tungsten roughing operation, the inhibitor of the tungsten roughing operation is compared with the inhibitor in the example 1 by using conventional carboxymethyl cellulose, and other medicament conditions are shown in the example 1. The comparative results of the mixed tungsten ore in the inhibitor test of tungsten roughing operation are shown in table 2.
Comparative example 3
The mixed tungsten ore of the same grade in the example 1 is subjected to tungsten roughing operation, the inhibitor of the tungsten roughing operation is compared with the inhibitor in the example 1 by using the conventional agent sodium hexametaphosphate, and other agent conditions are shown in the example 1. The comparative results of the mixed tungsten ore in the inhibitor test of tungsten roughing operation are shown in table 2.
TABLE 2 comparative test of mixed tungsten roughing operation inhibitor for tungsten ore
As can be seen from Table 2, the inhibitor of the present invention has the best inhibitory effect in the roughing operation as compared with the conventional inhibitor. By adopting the inhibitor, the grade of the tungsten rough concentrate reaches 12.23%, the recovery rate reaches 87.40%, and the beneficiation index is the best.
Comparative example 4
The mixed tungsten ore of the same grade in the example 1 is subjected to tungsten roughing operation, a collector in the tungsten roughing operation is compared with the collector in the example 1 by using a conventional medicament, namely hydroximic acid, and other medicament conditions are shown in the example 1. The comparative results of the collecting agent test of the mixed tungsten ore in the tungsten roughing operation are shown in the table 3.
Comparative example 5
The same grade mixed tungsten ore of example 1 was subjected to tungsten rougher flotation using a collector that was compared to the collector of example 1 using a conventional sulfated oleate soap, and other conditions were as described in example 1. The comparative results of the collecting agent test of the mixed tungsten ore in the tungsten roughing operation are shown in the table 3.
Comparative example 6
The mixed tungsten ore with the same grade in the example 1 is subjected to tungsten roughing operation, a collector in the tungsten roughing operation is compared with the collector in the example 1 by using a conventional reagent sodium oleate, and other reagent conditions are shown in the example 1. The comparative results of the collecting agent test of the mixed tungsten ore in the tungsten roughing operation are shown in the table 3.
TABLE 3 collecting agent contrast test for mixed tungsten roughing operation
As can be seen from Table 3, in the rough concentration operation of the mixed tungsten, the grade of the rough tungsten concentrate is higher and is 12.19%, the recovery rate reaches 87.66%, and the recovery rate is highest. The collecting agent has the best effect by comprehensively considering the grade and the recovery rate of rough tungsten concentrate in the roughing operation.
Claims (10)
1. A beneficiation method of mixed type refractory tungsten ore comprises the following steps:
firstly, grinding ore:
grinding the crushed black-white tungsten paragenetic ore raw ore to obtain ore pulp;
mixing tungsten for roughing:
adding 1000-1500 g/t of sodium carbonate into the ore pulp according to the dry weight of the crushed raw ore of the black-white tungsten paragenic ore until the pH value of the ore pulp is 7.0-9.0, and then adding 800-1200 g/t of an inhibitor, 500-600 g/t of an activating agent lead nitrate and 400-600 g/t of a collecting agent for mixed tungsten roughing to respectively obtain tungsten rough concentrate ore pulp and rough tailings ore pulp;
thirdly, scavenging with mixed tungsten:
performing two times of mixed tungsten scavenging operation on the rougher tailing pulp to obtain tungsten scavenging tailings I;
four weak magnetic iron removal operations:
carrying out magnetic separation on the tungsten rough concentrate ore pulp by adopting a permanent magnet drum type low intensity magnetic separator under the condition that the magnetic field intensity is 0.2T to respectively obtain a magnetic iron product and magnetic separation tailing ore pulp;
fifthly, performing strong magnetic separation on tungsten:
performing strong magnetic rough separation on the magnetic separation tailing pulp by adopting a high-gradient magnetic separator under the condition that the magnetic field intensity is 1.0-1.5T to respectively obtain black tungsten concentrate and strong magnetic separation tailing pulp; carrying out strong magnetic scavenging on the strong magnetic separation tailing pulp under the condition that the magnetic field intensity is 0.6-0.8T to respectively obtain magnetic separation middlings and scavenging operation tailings; the magnetic separation middling and the black tungsten concentrate are combined into a black tungsten concentrate product;
sixthly, performing dense dehydration:
concentrating and dehydrating the scavenging operation tailings to respectively obtain ore pulp and overflow water with the concentration of 60-70%;
scheelite flotation operation:
and performing scheelite roughing operation, scheelite scavenging operation and scheelite concentration operation on the ore pulp with the concentration of 60-70% to respectively obtain scheelite concentrate and tungsten scavenging tailings II.
2. The mixed type refractory tungsten ore dressing method according to claim 1, characterized in that: the conditions for grinding the ores in the step mean that the mass ratio of the crushed raw ores of the black-white tungsten paragenetic ores to water is 1: 1; according to the dry weight of the black and white tungsten paragenetic raw ore, the grinding fineness of the ground ore product is-74 mu m and accounts for 75-80%.
3. The mixed type refractory tungsten ore dressing method according to claim 1, characterized in that: the step three, twice mixed tungsten scavenging operation refers to adding 100-200 g/t of inhibitor and 80-120 g/t of collector into the rough concentration tailing pulp to perform once tungsten scavenging operation according to the dry ore weight of the crushed black-white tungsten paragenic ore raw ore, so as to obtain once scavenged tailing pulp and once scavenged middling respectively, and the once scavenged middling enters the mixed tungsten rough concentration; adding 50-80 g/t of inhibitor and 30-50 g/t of collecting agent into the primary scavenging tailing pulp to carry out secondary tungsten scavenging to respectively obtain the tungsten scavenging tailings I and secondary scavenging middlings, and returning the secondary scavenging middlings to the primary tungsten scavenging operation.
4. The mixed type refractory tungsten ore beneficiation method according to claim 1 or 3, wherein: the inhibitor is prepared by mixing water glass, sodium polyacrylate, sodium sulfite and sodium hexametaphosphate in a ratio of 2-4: 1: 1: 1, in a mass ratio of 1.
5. The mixed type refractory tungsten ore beneficiation method according to claim 1 or 3, wherein: the collecting agent is prepared by mixing hydroximic acids, fatty acids and glycerol monostearate according to the weight ratio of 1-2: 0.5-1.0: 0.3, and heating and stirring in a water bath for 0.5 to 1.0 hour under the conditions that the temperature is 30 to 50 ℃ and the stirring speed is 600 to 900 r/min.
6. The mixed type refractory tungsten ore dressing method according to claim 5, wherein: the hydroxamic acid is one or more of octyl hydroxamic acid, salicylhydroxamic acid and benzohydroxamic acid.
7. The mixed type refractory tungsten ore dressing method according to claim 5, wherein: the fatty acid is one or more of oleic acid, oxidized paraffin soap, sodium oleate and tall soap.
8. The mixed type refractory tungsten ore dressing method according to claim 1, characterized in that: the scheelite roughing operation in the step S-S is that 1500-2000 g/t of water glass and 733300-500 g/t of oxidized paraffin soap are added into ore pulp with the concentration of 60-70% according to the dry weight of the crushed raw ore of the black-white tungsten paragenic ore, then the ore pulp is heated to 85-95 ℃ and stirred for 60 minutes, and the scheelite rough concentrate ore pulp and the scheelite roughing tailing ore pulp are respectively obtained.
9. The mixed type refractory tungsten ore dressing method according to claim 1, characterized in that: the scheelite scavenging operation in the step-wise includes that collecting agent oxidized paraffin soap 73360-100 g/t is added into scheelite roughing tailing pulp to perform primary scavenging operation according to the dry weight of the crushed raw ore of the wolframite and wolframite, so that primary scheelite scavenging tailing pulp and primary scheelite scavenging middling are obtained respectively, and the primary scheelite scavenging middling enters the scheelite roughing operation; adding a collecting agent oxidized paraffin soap 73330-50 g/t into the primary scheelite scavenging tailing pulp to carry out secondary scavenging to obtain the tungsten scavenging tailing II and secondary scheelite scavenging middlings respectively, and returning the secondary scheelite scavenging middlings to the primary scavenging operation.
10. The mixed type refractory tungsten ore dressing method according to claim 1, characterized in that: the scheelite concentration operation in step-nickle is to perform concentration operation on scheelite rough concentrate pulp for four times according to a conventional method without adding any medicament to obtain scheelite concentrate; and the middlings in the first concentration enter the scheelite roughing operation, and the middlings in the second to fourth concentrations return to the previous operation cycle in sequence.
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Application publication date: 20210910 |