CN112642591B - Method for improving floatation recovery rate of kaolinite by using modified nano bubbles - Google Patents
Method for improving floatation recovery rate of kaolinite by using modified nano bubbles Download PDFInfo
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- CN112642591B CN112642591B CN202011599155.3A CN202011599155A CN112642591B CN 112642591 B CN112642591 B CN 112642591B CN 202011599155 A CN202011599155 A CN 202011599155A CN 112642591 B CN112642591 B CN 112642591B
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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
Abstract
The invention belongs to the technical field of kaolinite flotation, and discloses a method for improving the kaolinite flotation recovery rate by using modified nano bubbles. Adding deionized water into a water tank; preparing dodecylamine and hydrochloric acid into a collector solution containing dodecylamine cations according to a molar ratio of 1:1, adding the solution into a water tank, and fully stirring; and circulating the mixed aqueous solution in which the dodecylamine cations are dissolved in the water tank for a certain time by using a nano bubble generating device to prepare the positively charged modified nano bubbles. From the kaolinite flotation result, on the premise of the same amount of the collecting agent, the recovery rate of the modified nano-bubble water flotation is improved by 17.8% compared with the conventional water flotation, and is improved by 8.4% compared with the conventional nano-bubble water flotation, so that the method can obviously improve the flotation recovery efficiency of the kaolinite, which is an important nonmetallic mineral resource, and bring economic benefits to enterprises.
Description
Technical Field
The invention belongs to the technical field of kaolinite flotation, and particularly relates to a method for improving the flotation recovery rate of kaolinite by modifying nano bubbles by using a cationic collector, namely dodecylamine.
Background
Kaolinite, also known as "kaolin", is a typical clay mineral and an important non-metallic mineral resource, and is widely used in the field of preparation of materials such as paper making, ceramics, rubber and refractory materials. Furthermore, kaolinite is often associated as a gangue mineral in bauxite and hematite. Flotation is the most common means of recovering kaolinite from kaolin mill tailings and separating bauxite and hematite from kaolinite. Because of its fine particle size, the probability that kaolinite particles collide with and adhere to bubbles during flotation is low, and therefore, the kaolinite recovery efficiency is low under conventional flotation means.
When the kaolinite crystal is broken, two kinds of crystal faces with different properties are generated, one kind is a bottom face with permanent negative charges and is divided into a silicon-oxygen tetrahedron (001) face and an aluminum-oxygen octahedron (001) - ) Kneading; the other is an end face charged with a variable charge. Flaky kaolinite particlesIn the solution, the nano-silver nano-particles mainly exist in four forms of dispersion, bottom surface-bottom surface, end surface-bottom surface and end surface-end surface. The research of experts at home and abroad finds that the flotation behavior of kaolinite is closely related to the particle aggregation form: in acid ore pulp or under the condition of high ionic strength, kaolinite particles are aggregated to form a disordered three-dimensional structure, and flotation is improved along with the disordered three-dimensional structure. Therefore, how to change the aggregation form of the kaolinite particles in the ore pulp so as to enable the kaolinite particles to be better recycled becomes a breakthrough for improving the kaolinite flotation recovery rate at present.
A nanobubble is a tiny bubble with a diameter less than 1 μm. Research finds that after nano bubbles are introduced into a flotation system, the nano bubbles are preferentially attached to the surfaces of hydrophobic mineral particles, so that the hydrophobicity of the mineral surfaces is enhanced, and meanwhile, the agglomeration of fine mineral particles is promoted, and therefore, the nano bubbles become an important means for improving the flotation recovery rate of the fine mineral particles. However, because kaolinite is entirely electronegative and naturally hydrophilic, the improvement of the flotation efficiency of the micro-fine particle kaolinite by the negatively charged conventional nanobubbles is limited. Therefore, a new method for improving the kaolinite flotation recovery rate by using the surface-modified nano bubbles is needed.
Through the above analysis, the problems and defects of the prior art are as follows: (1) the technical scheme of combining the nano bubbles with the method for improving the floatation recovery rate of the kaolinite in the prior art is not reported yet.
(2) The particle size of the kaolinite is usually below 2 μm, and the kaolinite is low in probability of being captured by bubbles due to small particle size in the flotation process, so that the kaolinite is a big bottleneck limiting the efficiency of recovering the kaolinite by the conventional flotation method.
(3) In the acid ore pulp, the bottom surface with negative charge and the end surface with positive charge attract each other to lead the kaolinite particles to form disordered agglomerations which mainly take an end surface-bottom surface form in the solution, and the floatability of the kaolinite is improved along with the disordered agglomerations. However, flotation under a strongly acidic condition not only accelerates the corrosion of equipment but also may cause environmental pollution.
(4) Under the condition of high ionic strength, the kaolinite is agglomerated because the electric double layer on the surface is compressed and the electrostatic repulsion between particles is weakened, and the floatation recovery rate of the kaolinite is obviously improved. However, flotation under high ionic strength conditions can shorten equipment life and significantly increase operating costs in the plant.
(5) Although the nano bubbles are an important means for flotation of fine-particle minerals, the kaolinite is electronegative and naturally hydrophilic as a whole, so that the promotion effect of the conventional nano bubbles on the formation of a three-dimensional aggregation structure of kaolinite particles is limited, and further the improvement on the floatation recovery rate of the kaolinite is limited.
The difficulty in solving the above problems and defects is:
how to find a means to induce the agglomeration of kaolinite particles under natural pulp (pH and ionic strength) conditions and the formed kaolinite particle aggregation structure must be beneficial to improve its flotation recovery efficiency.
The significance of solving the problems and the defects is as follows:
the method changes the aggregation state of kaolinite particles in natural ore pulp by a new mild means, solves the problem of low recovery efficiency of fine-particle kaolinite in the traditional means of flotation, avoids negative effects possibly caused by high acidity or high ionic strength, and has relatively greater improvement on the recovery efficiency compared with the conventional nano-bubble flotation, which has important significance for efficiently recycling the kaolinite, namely an important non-metal mineral resource.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for improving the flotation recovery rate of kaolinite by using modified nano bubbles.
The invention is realized in such a way that a method for improving the flotation recovery rate of kaolinite by using modified nano bubbles comprises the following steps:
step one, adding deionized water into a water tank;
step two, preparing dodecylamine and hydrochloric acid into a collector solution containing dodecylamine cations according to a molar ratio of 1:1, adding the collector solution into a water tank, and stirring to fully dissolve the solution;
and step three, circulating the mixed aqueous solution containing the dodecylamine cations by using a nano bubble generating device to generate the positively charged modified nano bubbles in the solution.
Further, in the second step, cationic surfactant dodecylamine and hydrochloric acid are prepared into a collector solution according to a molar ratio of 1:1, the collector solution is added into the water tank, and the concentration of the collector solution obtained after mixing dodecylamine and hydrochloric acid in a system is 3 x 10 - 4 mol/L。
Further, when the three-purpose nanometer bubble generating device circulates the mixed water solution containing the dodecylamine cations, the water flow is 18L/min, the water pressure is 0.2Mpa, the air inflow is 0.18L/min, and the operation time is 5 min.
After the third step, the following steps are required:
(1) adding the kaolinite pure mineral and the positively-charged modified nano-bubble-enriched water into a flotation tank, and starting a flotation machine;
(2) in the stirred ore pulp, the electropositivity of the modified nano bubbles promotes the adsorption of the modified nano bubbles on the surface of the kaolinite, and the kaolinite particles with the nano bubbles attached to the surface form a disordered three-dimensional aggregation structure under the action of a nano bubble bridging force;
(3) stirring and scraping bubbles;
(4) two groups of comparison tests are carried out to obtain a kaolinite flotation time recovery rate relation graph under three different systems.
Further, the rotating speed of the impeller in the step (1) is 1680 r/min.
The stirring time of the flotation operation in the step (3) is 3 min; then, starting to scrape bubbles; the foam scraping time is 4 min.
The step (4) of carrying out two groups of control experiments comprises the following steps: the method is carried out in common deionized water and conventional nano bubble water, and the two groups of control experiment conditions are stirring for 3 min; then adding a lauryl amine solution with the same concentration; then stirring for 2 min; starting to scrape bubbles;
said step (4) of performing two control tests further comprises:
the two control experiments had a lather scraping time of 4 min.
The kaolinite flotation time recovery rate relational graph obtained in the step (4) under three different systems comprises the following steps: drying and weighing at 80 ℃ to obtain a kaolinite flotation time and recovery rate relation graph under three different systems.
Specifically, the flotation behaviors of kaolinite under three different systems are compared through flotation experiments, and the flotation recovery rates of kaolinite under three different systems are determined.
Further, the flotation behavior of kaolinite under three different systems is compared through a flotation experiment, and the flotation recovery rate of kaolinite under three different systems is determined, which comprises the following steps:
(1) adding 3.2g of kaolinite pure mineral and 40mL of water (deionized water, nano bubble water and modified nano bubble water) into a 50mL flotation tank, and stirring for 3 min;
(2) adding a collector solution into deionized water and nano bubble water during flotation until the concentration of dodecylamine in ore pulp is 3 multiplied by 10 -4 mol/L, adding the modified nano bubble water during flotation, stirring for 2min, and then starting scraping bubbles;
(3) drying and weighing at 80 ℃ to obtain a kaolinite flotation time recovery rate relation graph under three different systems.
Preferably, in the present invention, the conventional nanobubble preparation method: adding 18L of deionized water into a 20L water tank, starting the nano bubble generating device, regulating water flow and air inflow through a control valve, and keeping water flow of 18L/min, water pressure of 0.2Mpa, air inflow of 0.18L/min and running time of 5min in the pipeline. The difference is that the preparation method of the positively charged modified nano bubbles of the invention is that before the equipment is operated, the collector solution is dripped into the water tank until the concentration of the dodecylamine is 3 multiplied by 10 -4 mol/L, the other operating steps remaining the same as described above.
The electric property and the potential of the generated modified nano bubbles can be known through a Zeta potential diagram 5; the reliability of the preparation of the positively charged modified nanobubbles is proved.
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any other modifications or substitutions that can be easily conceived by those skilled in the art through the technical solution of the present invention, such as using positively charged modified nanobubbles to improve the flotation recovery efficiency of other clay minerals like muscovite and illite, etc., are also within the scope of the present invention.
The invention has the advantages and positive effects that:
the key point of the invention is that the modified nano-bubbles with positive charges are prepared by using a dodecylamine collecting agent solution and are introduced into a kaolinite flotation system, so that kaolinite particles in ore pulp are induced to aggregate to form a three-dimensional aggregation structure beneficial to kaolinite flotation, and the recovery rate is improved. The invention focuses on the mechanism, process and method for modifying the nano bubbles and the higher recovery rate of flotation by utilizing the modified nano bubbles compared with the conventional method.
Firstly, 18L of deionized water is added into a water tank with the volume of 20L as shown in figure 3, cationic surfactant lauryl amine and hydrochloric acid are prepared into collecting agent solution according to the molar ratio of 1:1, and the collecting agent solution is added into the water tank to ensure that the concentration of the medicinal agent reaches 3 x 10 -4 And (3) mol/L, stirring to fully dissolve the solution, and treating the aqueous solution containing dodecylamine cations by using a nano bubble generating device (through hydrodynamic cavitation) as shown in figure 3 to generate positively charged nano bubbles, wherein the specific setting parameters are as follows: the water flow is 18L/min, the water pressure is 0.2Mpa, the air inflow is 0.18L/min, and the operation time is 5 min.
Zeta potential test proves that the experimental method can modify the nano bubbles and charge the nano bubbles with positive electricity, and a Zeta potential test result graph is shown in figure 5.
Secondly, 3.2g of kaolinite pure mineral and 40mL of modified nano-bubble water are added into a 50mL flotation tank, the rotating speed of an impeller is 1680r/min, at the moment, in stirred ore pulp, the electropositivity of the modified nano-bubbles promotes the adsorption of the modified nano-bubbles on the surface of kaolinite, kaolinite particles with the nano-bubbles attached to the surface form a disordered three-dimensional aggregation structure under the action of a nano-bubble bridge force, and the flotation recovery rate is improved accordingly. The stirring time of the flotation operation is 3 min; then, starting to scrape bubbles; wherein the foam scraping time is 4 min; the other two groups of control tests are carried out in common deionized water and conventional nanobubble water, and the two groups of test conditions are stirring for 3min differently; then adding a lauryl amine collecting agent solution with the same concentration; then stirring for 2 min; starting to scrape bubbles; the foam scraping time of the three systems is the same; the pH value of the three systems is the same under the experimental conditions (the pH value is about 7) measured by a pH meter; drying and weighing at 80 ℃ to obtain kaolinite flotation time recovery rate relational graphs under three different systems.
According to the method for improving the flotation recovery rate of the kaolinite by using the modified nano bubbles, provided by the invention, by introducing the positively charged modified nano bubbles to carry out a series of researches on the kaolinite particles such as flotation, sedimentation, rheology, potential analysis and the like from the aspects of experiments and mechanisms under the condition of natural ore pulp, the positively charged modified nano bubbles are found to induce the kaolinite particles to agglomerate so as to strengthen the kaolinite flotation.
According to the invention, through comparison of kaolinite flotation behaviors in three different systems (a deionized water system, a nano bubble water system and a positively charged modified nano bubble water system), the kaolinite flotation recovery rate in the deionized water system is 67.8%, the kaolinite flotation recovery rate in the nano bubble water system is 76.2%, and the kaolinite flotation recovery rate in the positively charged modified nano bubble water system is 85.6%.
From the flotation recovery rate result, from the kaolinite flotation result, on the premise of the same amount of the collecting agent, the recovery rate of the modified nano-bubble water flotation is improved by 17.8% compared with the conventional water flotation, and the recovery rate of the modified nano-bubble water flotation is improved by 8.4% compared with the conventional nano-bubble water flotation, so that the method can obviously improve the flotation recovery efficiency of the kaolinite, which is an important nonmetallic mineral resource, and bring economic benefits to enterprises.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart of a method for improving kaolinite flotation recovery rate by using modified nano-bubbles according to an embodiment of the invention.
Fig. 2 is a schematic diagram of flotation experiments in three different systems provided by the embodiment of the invention.
Fig. 3 is a schematic view of a nanobubble generating device according to an embodiment of the present invention.
In fig. 3: 1. a pump; 2. a valve; 3. a pressure gauge; 4. an air inlet pipe; 5. a gas flow meter; 6. a nanobubble nozzle.
Figure 4 is a graph of kaolinite flotation time recovery under three different systems provided by examples of the present invention.
FIG. 5 is Zeta potential diagram of modified nanobubbles prepared by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a method for improving the flotation recovery rate of kaolinite by using modified nano bubbles, and the invention is described in detail by combining the attached drawings.
The method for improving the flotation recovery rate of the kaolinite by using the modified nano bubbles comprises the following steps: and comparing the flotation behaviors of the kaolinite under three different systems through flotation experiments to determine the flotation recovery rates of the kaolinite under the three different systems.
As shown in fig. 1, the present invention provides a method for improving the flotation recovery rate of kaolinite by using modified nanobubbles, wherein the method for improving the flotation recovery rate of kaolinite by using modified nanobubbles comprises:
s101, adding deionized water into a water tank;
s102, preparing dodecylamine and hydrochloric acid into a collector solution containing dodecylamine cations according to a molar ratio of 1:1, adding the collector solution into a water tank, and stirring to fully dissolve the solution;
and S103, circulating the mixed aqueous solution containing the dodecylamine cations by using a nano bubble generating device to generate the positively charged modified nano bubbles in the solution.
Step S102, cationic surfactant dodecylamine and hydrochloric acid are prepared according to a molar ratio of 1:1Adding collector solution into a water tank, wherein the concentration of the collector solution in a system obtained by mixing dodecylamine and hydrochloric acid is 3 multiplied by 10 -4 mol/L。
In the step S103, when the mixed aqueous solution containing the dodecylamine cations is circulated by using the nano-bubble generating device, the water flow is 18L/min, the water pressure is 0.2Mpa, the air inflow is 0.18L/min, and the operation time is 5 min.
After step S103, the following steps are also performed:
(1) adding the kaolinite pure mineral and the positively-charged modified nano-bubble-enriched water into a flotation tank, and starting a flotation machine;
(2) in the stirred ore pulp, the electropositivity of the modified nano bubbles promotes the adsorption of the modified nano bubbles on the surface of the kaolinite, and the kaolinite particles with the nano bubbles attached to the surface form a disordered three-dimensional aggregation structure under the action of a nano bubble bridging force;
(3) stirring and scraping bubbles;
(4) two groups of comparison tests are carried out to obtain a kaolinite flotation time recovery rate relation graph under three different systems.
The rotating speed of the impeller in the step (1) is 1680 r/min.
The stirring time of the flotation operation in the step (3) is 3 min; then, starting to scrape bubbles; the foam scraping time is 4 min.
The step (4) of carrying out two groups of control experiments comprises the following steps: the method is carried out in common deionized water and conventional nano bubble water, and the two groups of control experiment conditions are stirring for 3 min; then adding a lauryl amine solution with the same concentration; then stirring for 2 min; starting to scrape bubbles;
said step (4) of performing two control tests further comprises:
the two control experiments had a lather scraping time of 4 min.
The kaolinite flotation time recovery rate relational graph obtained in the step (4) under three different systems comprises the following steps: drying and weighing at 80 ℃ to obtain a kaolinite flotation time recovery rate relation graph under three different systems.
Preferably, the method for determining the flotation recovery rate of kaolinite in three different systems by comparing the flotation behaviors of kaolinite in three different systems through flotation experiments provided by the embodiment of the invention comprises the following steps:
adding 3.2g of kaolinite pure mineral and 40mL of water (deionized water, nano bubble water and modified nano bubble water) into a 50mL flotation tank, and stirring for 3 min;
adding a collector solution into deionized water and nano bubble water during flotation till the concentration of dodecylamine in ore pulp is 3 multiplied by 10 - 4 mol/L, adding the modified nano bubble water during flotation, stirring for 2min, and then starting scraping bubbles; wherein the foam scraping time is 4 min;
drying and weighing to obtain a kaolinite flotation time recovery rate relation chart under three different systems.
Claims (8)
1. The method for improving the flotation recovery rate of kaolinite by using the modified nano bubbles is characterized by comprising the following steps:
step one, adding deionized water into a water tank;
preparing a cationic surfactant dodecylamine and hydrochloric acid into a collector solution containing dodecylamine cations according to a molar ratio of 1:1, adding the collector solution into a water tank, and stirring to fully dissolve the solution;
the concentration of the collector solution obtained after mixing the dodecylamine and the hydrochloric acid in the system is 3 multiplied by 10 -4 mol/L；
Circulating the mixed aqueous solution containing the dodecylamine cations by using a nano bubble generating device to generate positively charged modified nano bubbles in the solution; then the following steps are carried out:
(1) adding kaolinite pure minerals and positively charged modified nano bubble water into a flotation tank, and starting a flotation machine;
(2) in the stirred ore pulp, the electropositivity of the modified nano bubbles promotes the adsorption of the modified nano bubbles on the surface of the kaolinite, and the kaolinite particles with the nano bubbles attached to the surface form a disordered three-dimensional aggregation structure under the action of a nano bubble bridging force;
(3) stirring and scraping bubbles;
(4) two groups of comparison tests are carried out to obtain a kaolinite flotation time recovery rate relation graph under three different systems.
2. The method for improving the flotation recovery rate of kaolinite according to claim 1, wherein when the step three-way nanobubble generation device circulates the mixed aqueous solution containing the dodecylamine cations, the water flow is 18L/min, the water pressure is 0.2MPa, the air inflow is 0.18L/min, and the operation time is 5 min.
3. The method for improving the flotation recovery of kaolinite according to claim 1, wherein the impeller rotation speed of step (1) is 1680 r/min.
4. The method for improving the flotation recovery rate of kaolinite according to claim 1, wherein the step (3) of flotation operation is performed for a stirring time of 3 min; then, starting to scrape bubbles; the foam scraping time is 4 min.
5. The method for improving the flotation recovery of kaolinite according to claim 1, wherein the step (4) of performing two control experiments comprises: the method is carried out in common deionized water and conventional nano bubble water, and the two groups of control experiment conditions are stirring for 3 min; then adding a collecting agent solution with the same concentration as that of the modified nano bubble water in the flotation process; then stirring for 2 min; the bulb scraping is started.
6. The method for improving kaolinite flotation recovery using modified nanobubbles of claim 5, wherein said step (4) of performing two control runs further comprises:
the two control experiments had a lather scraping time of 4 min.
7. The method for improving kaolinite flotation recovery using modified nanobubbles of claim 5, wherein said step (4) of obtaining a kaolinite flotation time recovery relationship plot for three different systems comprises: drying and weighing at 80 ℃ to obtain a kaolinite flotation time recovery rate relation graph under three different systems.
8. An apparatus for improving the flotation recovery rate of kaolinite by implementing the method for improving the flotation recovery rate of kaolinite by using the modified nanobubbles according to any one of claims 1 to 7.
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