CN112676043B - Method for improving heating flotation effect of scheelite - Google Patents
Method for improving heating flotation effect of scheelite Download PDFInfo
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Abstract
The invention discloses a method for improving the warming flotation effect of scheelite, which uses 2D layered MoS in the warming flotation of the scheelite2The nano-sheet is used as a desoxidant. This novel 2D layered MoS2When the nanosheet is used as a flotation reagent, the nanosheet has a large specific surface and rich active sites, so that the nanosheet can adsorb a residual reagent in the rough flotation of scheelite, remove the influence of the residual reagent on the warming flotation of the scheelite and greatly improve the separation effect of the warming flotation of the scheelite; meanwhile, sulfur atoms in the molecules of the scheelite flotation agent can perform a complex reaction with metal ions in water, so that the influence of inevitable metal ions in water on flotation is eliminated, the heating flotation effect of the scheelite is improved, and the flotation efficiency and recovery rate of the scheelite concentration by heating are effectively improved.
Description
Technical Field
The invention belongs to the technical field of mineral separation, and particularly relates to a method for improving the heating flotation effect of scheelite.
Background
Tungsten metal has a wide range of uses in the industrial field and is being used as a strategic reserve resource by countries in the world due to its scarcity and irreplaceability. Scheelite is closely symbiotic with calcium-containing gangue minerals such as calcite and fluorite, has similar physical and chemical properties with gangue in the aspects of hardness, relative specific gravity, solubility and the like, particularly has calcium ions as surface positioning ions, and shows similar adsorption behavior in the interaction with a collecting agent; meanwhile, the scheelite has low hardness and is easy to over-crush, and in a scheelite flotation solution system, coarse grains and fine grains and different minerals have interaction, so that the flotation separation of the scheelite and the calcium-containing gangue minerals is difficult. A large number of researches and production practices show that the scheelite usually needs normal temperature-heating two-stage flotation to obtain high-grade tungsten concentrate, namely, the scheelite is subjected to normal temperature flotation to obtain scheelite rough concentrate, and then the scheelite is subjected to heating flotation to obtain the high-grade scheelite concentrate by adopting a 'Pedelov' method. The 'Pedelov method' is that concentrated rough concentrate is added with a large amount of desiccants (water glass) under the condition of high temperature to be stirred for a long time with high strength and then subjected to slurry-mixing flotation, under the condition, oleic acid adsorbed on the surface of positively charged calcite is fully resolved due to strong competitive adsorption of the high-concentration desiccants and causes inhibition, and scheelite with negative charges on the surface is slightly influenced by the desiccants and can still continuously keep the chemical adsorption with the oleic acid, so that the good floatability can be still kept, and the aim of separating the scheelite from gangue minerals is fulfilled. The process has stable production indexes, but has relatively high energy consumption and ore dressing cost. Therefore, the development of a new process and a new medicament for efficiently recovering the scheelite resource have positive significance for maintaining the sustainable development of the tungsten industry in China.
Molybdenum disulfide (MoS)2) Is a typical transition metal sulfide and has a graphene-like structure. Nano-sized MoS2The nano-composite material has the advantages of large specific surface area, strong adsorption capacity, high reaction activity, adjustable energy band width and the like, has wide application prospect in the fields of nano-electronics, optoelectronics, gas-sensitive sensing and the like, and draws wide attention of researchers. Molybdenum disulfide (MoS)2) As a novel nano material, the nano material has larger specific surface area, higher carrier migration rate and low noise level, MoS2Is a typical transition metal sulfide and consists of an S-Mo-S three-layer sandwich structure, wherein the layers are combined through stronger covalent bonds, the Van der Waals force between the layers is weaker, and the combination force is weaker and can be stripped into single-layer or multi-layer nano sheetsAnd (3) layer structure. Due to the ultrathin planar structure, the two-dimensional 2D layered molybdenum disulfide nanosheet has a quantum size effect, can limit electrons in an ultrathin plane with atomic thickness, and is sensitive to signals of surrounding environments such as electricity, light, heat and the like. Compared with graphene (zero band gap) and graphene oxide, the two-dimensional 2D layered molybdenum disulfide nanosheet has a direct band gap, and has wider application in the fields of electronics, photoelectricity and the like than graphene. In recent years, two-dimensional 2D layered molybdenum disulfide nanosheets have played a role in a variety of fields such as food detection, medical diagnosis, biological analysis, environmental monitoring, and the like.
Currently, there are 2D layered MoS2The application of the nanosheets in scheelite warming flotation is not reported.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a method for improving the scheelite warming flotation effect, and solves the problems of poor scheelite concentrate grade and recovery rate, especially large water glass consumption and high cost, caused by large water glass consumption, high cost and poor scheelite and gangue mineral separation effect of the existing scheelite warming flotation process.
In order to solve the technical problems, the invention adopts the technical scheme that:
a method for improving the heating flotation effect of scheelite comprises the following steps:
step 1, concentrating the scheelite rough concentrate to 55-60% of concentration by a thickener to obtain concentrated scheelite rough concentrate grit;
step 2, heating the concentrated scheelite rough concentrate sand sediment obtained in the step 1 to 50-55 ℃, and then adding 2D layered MoS2Nanosheet stirring; then, continuously heating to 65-70 ℃, adding 733 parts of oxidized paraffin soap, and stirring; then continuously heating to 75-80 ℃, adding sodium hydroxide, and stirring; then continuously heating to 85-90 ℃, adding water glass, and stirring; then continuously heating to 95-100 ℃, and stirring for 15 minutes to obtain heated rough concentrate;
and 3, adding water into the heated rough concentrate obtained in the step 2 to dilute the rough concentrate to a concentration of 30-40%, and then performing a flotation process without adding any reagent to obtain the scheelite concentrate.
Further, WO in the scheelite rough concentrate in the step 13The content of the mineral is 3% -10%, the granularity of the mineral is-200 meshes and accounts for 80% -90%, and the pH value of the ore pulp is 8-10.
Further, the 2D layered MoS in step 22The thickness of the nano-sheet is 1 nm-4 nm, and the diameter is 50 nm-200 nm.
Further, 2D layered MoS in step 22The dosage of the nano sheet is 100 g/t-200 g/t, and the stirring time is 3 minutes.
Further, the amount of the oxidized paraffin soap 733 in step 2 was 500g/t to 600g/t, and the stirring time was 5 minutes.
Furthermore, the dosage of the sodium hydroxide in the step 2 is 2000 g/t-3000 g/t, and the stirring time is 4 minutes.
Furthermore, the dosage of the water glass in the step 2 is 15 kg/t-20 kg/t, and the stirring time is 10 minutes.
Further, the flotation process in the step 3 comprises one roughing, two concentrating and two scavenging.
After the technical scheme is adopted, compared with the prior art, the invention has the following beneficial effects.
(1) Novel 2D layered MoS2When the nanosheet is used as a flotation reagent, the nanosheet has a large specific surface and rich active sites, so that the nanosheet can adsorb a residual reagent in the scheelite roughing flotation, the influence of the residual reagent on the scheelite warming flotation is removed, the problem of poor separation effect of scheelite and gangue minerals in the scheelite warming flotation is greatly improved, and the using amount of water glass is greatly reduced.
(2) Novel 2D layered MoS2The sulfur atoms in the molecules of the nano sheets can perform a complex reaction with metal ions in water, so that the influence of inevitable metal ions in water on flotation is eliminated, the heating flotation effect of scheelite is improved, and the flotation efficiency and recovery rate of scheelite heating concentration are effectively improved.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention to its proper form. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a schematic flow diagram of the process of the present invention;
it should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
The invention provides a method for improving the scheelite warming flotation effect, aiming at the problems of poor scheelite concentrate grade and recovery rate, especially large water glass consumption and high cost caused by large water glass consumption, high cost and poor scheelite and gangue mineral separation effect of the existing scheelite warming flotation process.
A method for improving the warming flotation effect of scheelite, which comprises the following steps (shown in the attached figure 1):
concentrating the scheelite rough concentrate to 55-60% by a thickener, wherein WO in the scheelite rough concentrate is3The content of the mineral is 3-10%, the granularity of the mineral is-200 meshes and accounts for 80-90%, and the pH value of the ore pulp is 8-10;
secondly, the temperature of the concentrated scheelite rough concentrate sand sediment obtained in the step I is raised to 50-55 ℃, and then 2D layered MoS is added2Nanosheet, 2D layered MoS2The thickness of the nano-sheet is 1 nm-4 nm,2D layered MoS with diameter of 50-200 nm2The dosage of the nano sheet is 100 g/t-200 g/t, and the stirring is carried out for 3 minutes; then, continuously heating to 65-70 ℃, adding oxidized paraffin soap 733, wherein the dosage of the oxidized paraffin soap 733 is 500-600 g/t, and stirring for 5 minutes; then continuously heating to 75-80 ℃, adding sodium hydroxide with the dosage of 2000-3000 g/t, and stirring for 4 minutes; then continuously heating to 85-90 ℃, adding water glass, wherein the using amount of the water glass is 15-20 kg/t, and stirring for 10 minutes; then continuously heating to 95-100 ℃, and stirring for 15 minutes;
and thirdly, adding water into the heated rough concentrate obtained in the second step to dilute the rough concentrate to a concentration of 30-40%, and then performing a flotation process flow of one-coarse-two-fine-sweeping, wherein no chemical is added in the flotation process to obtain the scheelite concentrate.
Example 1:this example is the 2D layered MoS2An application example of the nano-sheet in scheelite heating floatation.
Aiming at a certain scheelite rough concentrate in Hunan, the method comprises the following steps: concentrating the scheelite rough concentrate to 57% by a thickener, wherein the scheelite rough concentrate contains WO3The content of the mineral is 7 percent, the granularity of the mineral is 85 percent with-200 meshes, and the pH value range of the ore pulp is 9; secondly, heating the concentrated scheelite rough concentrate sand sediment obtained in the step I to 53 ℃, and then adding 2D layered MoS2Nanosheet, 2D layered MoS2The dosage of the nano sheets is 150g/t, and the stirring is carried out for 3 minutes; then, continuously heating to 67 ℃, adding oxidized paraffin soap 733, wherein the dosage of the oxidized paraffin soap 733 is 550g/t, and stirring for 5 minutes; then, continuously heating to 77 ℃, adding sodium hydroxide with the dosage of 2500g/t, and stirring for 4 minutes; then, continuously heating to 87 ℃, adding water glass, wherein the using amount of the water glass is 17kg/t, and stirring for 10 minutes; then, the temperature is continuously increased to 97 ℃, and the mixture is stirred for 15 minutes; and thirdly, adding water into the heated rough concentrate obtained in the second step to dilute the heated rough concentrate to a concentration of 35%, and then performing a flotation process flow of one-step coarse flotation, two-step fine flotation and two-step fine flotation without adding any reagent in the flotation process to obtain the scheelite concentrate. Novel 2D layered MoS in the invention2The comparative test results of the nanosheet and the common scheelite warming flotation process (the dosage of the water glass is 50kg/t) are shown in the table1. As can be seen from Table 1, compared with the conventional scheelite warming flotation process (the amount of water glass is 50kg/t), the novel 2D layered MoS is adopted2Nanosheet, WO in scheelite concentrate3The recovery rate is improved by 11.08 percent, WO3The grade of the product is improved by 3.56 percentage points, and the consumption of the water glass is reduced by 33 kg/t.
TABLE 1 scheelite flotation by warming comparative test results
Example 2:this example is the 2D layered MoS2Another application example of the nano-sheet in the scheelite warming flotation.
Aiming at a certain scheelite rough concentrate in the west of the river, the following steps are adopted: concentrating the scheelite rough concentrate to 55% by a thickener, wherein WO in the scheelite rough concentrate3The content of the mineral is 3 percent, the granularity of the mineral is-200 meshes and accounts for 80 percent, and the pH value range of the ore pulp is 8; secondly, heating the concentrated scheelite rough concentrate sand sediment obtained in the step I to 50 ℃, and then adding 2D layered MoS2Nanosheet, 2D layered MoS2The dosage of the nano sheet is 100g/t, and the stirring is carried out for 3 minutes; then, continuously heating to 65 ℃, adding the oxidized paraffin soap 733, wherein the dosage of the oxidized paraffin soap 733 is 500g/t, and stirring for 5 minutes; then, continuously heating to 75 ℃, adding sodium hydroxide with the dosage of 2000g/t, and stirring for 4 minutes; then, continuously heating to 85 ℃, adding water glass, wherein the using amount of the water glass is 15kg/t, and stirring for 10 minutes; then, continuously heating to 95 ℃, and stirring for 15 minutes; and thirdly, adding water into the heated rough concentrate obtained in the second step to dilute the heated rough concentrate to a concentration of 30%, and then performing a flotation process flow of one-step coarse flotation, two-step fine flotation and two-step fine flotation without adding any reagent in the flotation process to obtain the scheelite concentrate. The obtained scheelite concentrate contains WO368.84% and the recovery rate is 93.97%.
Example 3:this example is the 2D layered MoS2Another application example of the nano-sheet in the scheelite warming flotation.
Aiming at a certain scheelite rough concentrate in YunnanThe method comprises the following steps: concentrating the scheelite rough concentrate to 56% by a thickener, wherein the scheelite rough concentrate contains WO3The content of the mineral is 4 percent, the granularity of the mineral is-200 meshes and accounts for 82 percent, and the pH value range of the ore pulp is 8; secondly, heating the concentrated scheelite rough concentrate sand sediment obtained in the step I to 51 ℃, and then adding 2D layered MoS2Nanosheet, 2D layered MoS2The dosage of the nano-sheets is 120g/t, and the stirring is carried out for 3 minutes; then, continuously heating to 66 ℃, adding oxidized paraffin soap 733, wherein the dosage of the oxidized paraffin soap 733 is 590g/t, and stirring for 5 minutes; then, continuously heating to 76 ℃, adding sodium hydroxide with the dosage of 2300g/t, and stirring for 4 minutes; then, continuously heating to 88 ℃, adding water glass, wherein the using amount of the water glass is 18kg/t, and stirring for 10 minutes; then, the temperature is continuously increased to 98 ℃, and the mixture is stirred for 15 minutes; and thirdly, adding water into the heated rough concentrate obtained in the second step to dilute the heated rough concentrate to a concentration of 37%, and then performing a flotation process flow of one-step coarse flotation, two-step fine flotation and two-step fine flotation without adding any reagent in the flotation process to obtain the scheelite concentrate. Novel 2D layered MoS in the invention2The comparative test results of the nanosheet and the common scheelite warming flotation process (the using amount of the water glass is 59kg/t) are shown in Table 1. As can be seen from Table 1, compared with the conventional scheelite warming flotation process (the amount of water glass is 59kg/t), the novel 2D layered MoS is adopted2Nanosheet, WO in scheelite concentrate3The recovery rate is improved by 8.78 percentage points, WO3The grade of the product is improved by 0.26 percentage point, and the consumption of the water glass is reduced by 41 kg/t.
TABLE 1 scheelite flotation by warming comparative test results
Example 4:this example is the 2D layered MoS2Another application example of the nano-sheet in the scheelite warming flotation.
Aiming at a scheelite rough concentrate in Gansu, the method comprises the following steps: concentrating the scheelite rough concentrate to 60% by a thickener, wherein WO in the scheelite rough concentrate3Content of (2) is 10%, ore particle size90 percent of-200 meshes, and the pH value range of the ore pulp is 10; secondly, heating the concentrated scheelite rough concentrate sand sediment obtained in the step I to 55 ℃, and then adding 2D layered MoS2Nanosheet, 2D layered MoS2The dosage of the nano-sheets is 200g/t, and the stirring is carried out for 3 minutes; then, continuously heating to 70 ℃, adding oxidized paraffin soap 733, wherein the dosage of the oxidized paraffin soap 733 is 600g/t, and stirring for 5 minutes; then, continuously heating to 80 ℃, adding sodium hydroxide with the dosage of 3000g/t, and stirring for 4 minutes; then, continuously heating to 90 ℃, adding water glass, wherein the using amount of the water glass is 20kg/t, and stirring for 10 minutes; then, continuously heating to 100 ℃, and stirring for 15 minutes; and thirdly, adding water into the heated rough concentrate obtained in the second step to dilute the heated rough concentrate to a concentration of 40%, and then performing a flotation process flow of one-step coarse flotation, two-step fine flotation and two-step fine flotation without adding any reagent in the flotation process to obtain the scheelite concentrate. The obtained scheelite concentrate contains WO369.92% and the recovery rate is 96.38%.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A method for improving the heating flotation effect of scheelite is characterized by comprising the following steps:
step 1, concentrating the scheelite rough concentrate to 55-60% of concentration by a thickener to obtain concentrated scheelite rough concentrate grit;
step 2, heating the concentrated scheelite rough concentrate sand sediment obtained in the step 1 to 50-55 ℃, and then adding 2D layered MoS2Nanosheet stirring; then, continuously heating to 65-70 ℃, adding 733 parts of oxidized paraffin soap, and stirring; then continue toHeating to 75-80 ℃, adding sodium hydroxide, and stirring; then continuously heating to 85-90 ℃, adding water glass, and stirring; then continuously heating to 95-100 ℃, and stirring for 15 minutes to obtain heated rough concentrate;
and 3, adding water into the heated rough concentrate obtained in the step 2 to dilute the rough concentrate to a concentration of 30-40%, and then performing a flotation process without adding any reagent to obtain the scheelite concentrate.
2. The method for improving the warming flotation effect of the scheelite according to claim 1, which is characterized in that: WO in scheelite rough concentrate in step 13The content of the mineral is 3% -10%, the granularity of the mineral is-200 meshes and accounts for 80% -90%, and the pH value of the ore pulp ranges from 8 to 10.
3. The method for improving the warming flotation effect of the scheelite according to claim 1, which is characterized in that: the 2D layered MoS in step 22The thickness of the nano-sheet is 1 nm-4 nm, and the diameter is 50 nm-200 nm.
4. The method for improving the warming flotation effect of the scheelite according to claim 1, which is characterized in that: 2D layered MoS in step 22The dosage of the nano sheet is 100 g/t-200 g/t, and the stirring time is 3 minutes.
5. The method for improving the warming flotation effect of the scheelite according to claim 1, which is characterized in that: the dosage of the oxidized paraffin soap 733 in the step 2 is 500 g/t-600 g/t, and the stirring time is 5 minutes.
6. The method for improving the warming flotation effect of the scheelite according to claim 1, which is characterized in that: in the step 2, the dosage of the sodium hydroxide is 2000 g/t-3000 g/t, and the stirring time is 4 minutes.
7. The method for improving the warming flotation effect of the scheelite according to claim 1, which is characterized in that: the dosage of the water glass in the step 2 is 15 kg/t-20 kg/t, and the stirring time is 10 minutes.
8. The method for improving the warming flotation effect of the scheelite according to claim 1, which is characterized in that: the flotation process in the step 3 comprises one-time rough concentration, two-time fine concentration and two-time scavenging.
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