CN115780094A - Low-temperature-resistant spodumene flotation collector and preparation method and application thereof - Google Patents
Low-temperature-resistant spodumene flotation collector and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a low-temperature-resistant spodumene flotation collector, and a preparation method and application thereof. The collector comprises oleic acid, tall oil, sodium alkyl benzene sulfonate and an emulsifier. The preparation method of the flotation collector comprises the following steps: heating oleic acid, mixing with tall oil, stirring and mixing uniformly, then adding sodium alkyl benzene sulfonate and mixing uniformly to obtain a mixed material, adding an emulsifier into the mixed material, and stirring until the reaction is complete to obtain the oil-in-oil emulsion. The collecting agent disclosed by the invention is wide in material source and low in price, the problem of dispersion of the spodumene collecting agent in ore pulp is solved by compounding oleic acid, tall oil and sodium alkyl benzene sulfonate, and the collecting agent has good collecting capability and selectivity in low-temperature ore pulp, so that the grade and the recovery rate of spodumene concentrate are improved, and the fluctuation of a flotation index caused by temperature change is reduced; the collector has good adaptability to various spodumene ores in different altitude areas, and is also beneficial to improving the grade and the recovery rate of spodumene and stabilizing the flotation indexes of a dressing plant.
Description
Technical Field
The invention relates to a low-temperature-resistant spodumene flotation collector, a preparation method and application thereof, and belongs to the technical field of mineral processing.
Background
Lithium is an indispensable key raw material for the development of the new energy automobile industry, the strategic position and the importance of the lithium are realized, and the safe supply of lithium resources is in healthy and stable development of strategic emerging industries such as the new energy automobile industry, energy storage, electronic information and the like. With the improvement of living standard of people and the more and more obvious tendency of urbanization, the proportion of high-end product yield of new energy vehicles is expected to be further improved in the future, and the required lithium material is derived from spodumene as a high-nickel ternary material for new energy vehicle supply, which means that the increase of the demand of the spodumene exceeds the average level of lithium resources.
Due to the influence factors of technology, mining cost and the like, the hard rock lithium is mainly granite pegmatite spodumene ore in Xinjiang and Sichuan and alkaline feldspar granite spodumene ore in Jiangxi at present. And the exploitation site of the granite pegmatite spodumene is mostly in the high-cold high-altitude area.
The existing spodumene flotation can achieve a good flotation effect only under a specific temperature condition, and because the collecting agent used in the traditional spodumene flotation is a fatty acid collecting agent, the collecting agent is sensitive to the flotation temperature, and the solubility and the dispersibility of the collecting agent in water at the temperature lower than 18 ℃ can be deteriorated, so that the collecting performance of the agent can be reduced. Therefore, in autumn and winter, the water temperature is lower than 18 ℃ for spodumene flotation, the ore pulp needs to be heated for flotation, even the ore pulp of some high-altitude separation plants needs to be heated for a long time, the flotation energy consumption is large, and the ore separation cost is increased.
Therefore, in order to overcome the defects of poor solubility, poor selectivity, sensitivity to low temperature, large medicament dosage, low concentrate recovery rate and the like of the traditional fatty acid collecting agent, an efficient low-temperature-resistant spodumene flotation collecting agent is urgently needed.
Disclosure of Invention
Technical problem to be solved
In order to solve the problems in the prior art, the invention provides a low-temperature-resistant spodumene flotation collector, and a preparation method and application thereof.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
the low temperature resistant spodumene flotation collector comprises, by weight, 55-60 parts of oleic acid, 22-28 parts of tall oil, 3-5 parts of sodium alkyl benzene sulfonate and 12-16 parts of an emulsifier.
The low-temperature-resistant spodumene flotation collector preferably has the structural general formula of R-
-SO 3 Na, wherein the R group is a non-polar group, preferably a hydrocarbon chain, the number of carbons in the non-polar group being from 12 to 18, i.e. R = C12 to C18.
Further, most preferably, the sodium alkyl benzene sulfonate is selected from sodium alkyl benzene sulfonates having nonpolar groups containing 12, 14, 16, and 18 carbon atoms.
The low-temperature-resistant spodumene flotation collector is preferably prepared by one or more of polyoxyethylene ether sorbitan fatty acid ester (T-80), sorbitan monooleate (S-80) and triethanolamine.
Further most preferably, the emulsifier is a mixture of 5.3-5.8: 8.3-9.1: 0.8-1 polyoxyethylene ether sorbitan fatty acid ester (T-80): sorbitan monooleate (S-80): a mixture of triethanolamine.
Preferably, the low temperature resistant spodumene flotation collector comprises 57.2 parts of oleic acid, 24.5 parts of tall oil, 3.9 parts of sodium alkyl benzene sulfonate, 14.4 parts of emulsifier and sodium dodecyl benzene sulfonate.
The oleic acid can adopt commercially available industrial plant oleic acid, and the iodine value of the oleic acid is 130-180; the tall oil can be crude tall oil obtained from paper making industry.
The preparation method of the low temperature resistant spodumene flotation collector preferably comprises the following steps:
A. adding oleic acid into a reaction kettle, heating to 40-50 ℃, slowly adding tall oil, stirring, adding sodium alkyl benzene sulfonate under the heating condition of 55-65 ℃, stirring until the sodium alkyl benzene sulfonate is completely dissolved, and fully and uniformly mixing;
B. and adding an emulsifier into the uniformly mixed materials, and continuously stirring to obtain brown oily matter, namely the low-temperature-resistant spodumene flotation collector.
In the preparation method, preferably, in the step A, the time for stirring twice is 20-30 min; in the step B, the mixture is continuously stirred for 30 to 60min at the stirring speed of 200 to 500r/min.
The application of the low-temperature-resistant spodumene flotation collector in the spodumene flotation is preferably characterized in that the temperature of the added water for flotation is 0-40 ℃; the temperature of the flotation pulp is 10-40 ℃, and the flotation pulp can be suitable for the low temperature of 10-20 ℃; the dosage of the flotation collector is 400-2000 g/t, and the most preferable dosage is 600-1200 g/t.
A process for flotation of spodumene comprising the steps of:
s1, grinding the spodumene raw ore, wherein the grinding fineness is 70-75% of-200 meshes, and adding water to obtain ore pulp;
s2, adding a pH regulator and an activating agent into the ore pulp, regulating the pH to 11-13, adding the flotation collecting agent to perform aerated flotation, scraping bubbles to obtain spodumene rougher foam, and collecting the bottom of a tank to obtain scavenging ore pulp;
and S3, carrying out blank concentration on spodumene rough concentration foam to obtain spodumene concentrate.
In the method as described above, preferably, in step S1, sodium carbonate is added to the spodumene raw ore or ore pulp in an amount such that the pH of the ore pulp is adjusted to 8.0 to 8.5; the amount of water added is 45% of the weight concentration of the ore pulp.
In the method, preferably, in step S1, naphthenic acid soap is added into the ore pulp according to 30-40 g/t of raw ore, the mixture is stirred for 2-3 min and then subjected to air flotation, and the froth scraping is carried out to obtain the easily floating impurities, wherein the bottom of the tank is spodumene ore pulp.
In the method, preferably, in step S2, the pH regulator is sodium hydroxide and is added in an amount to make the pH value of the ore pulp be 11 to 13; the activator is calcium chloride, and the addition amount is 0-150 g/t raw ore; the stirring time is 25-35 min, and the stirring speed is 1900-2000 r/min.
In the method, preferably, in step S2, after stirring, the concentration of the ore slurry is adjusted to 30%, a flotation collector is added, the amount of the collector is 400-2000 g/t, and when the flotation collector is added, the flotation collector is firstly prepared into an aqueous solution with the weight percentage concentration of 5-10% and then added.
Further, the dosage of the flotation collector is 600-1200 g/t based on raw ore.
Preferably, in the step S3, the blank concentration is only to add water without adding any reagent, and the blank concentration is divided into two times, wherein the pulp concentration of the first-stage blank concentration needs to be adjusted to 15-20%, the pulp is stirred for 2min and then blown by air, and the pulp concentration of the second-stage blank concentration is 10-15%.
The blank concentration is a process that the gangue minerals in the rough concentrate are further thrown away by using the residual agent of the ore pulp and the stirring aeration performance of the flotation machine in the low-concentration ore pulp, the useful minerals are further enriched, and the grade of the concentrate is improved, wherein the blank concentration is preferably performed twice or more.
The method preferably further comprises S4, adding the scavenged ore pulp into the flotation collector in an amount of 30-200 g/t according to the raw ore, stirring, performing air flotation, wherein the scavenged foam product is scraped, and the spodumene flotation tailings are arranged at the bottom of the tank.
(III) advantageous effects
The invention has the beneficial effects that:
the low-temperature-resistant spodumene flotation collector provided by the invention has strong collecting capability and selectivity under a low-temperature condition, has good adaptability to various spodumenes in different altitude areas, and can stabilize flotation indexes of a concentrating mill.
The low-temperature-resistant spodumene flotation collector provided by the invention comprises oleic acid, tall oil, sodium dodecyl benzene sulfonate and an emulsifier as raw materials, and has the advantages of wide raw material source, stable property, low price and low cost.
The low-temperature-resistant spodumene flotation collector disclosed by the invention is mild in preparation conditions, good in stability and suitable for mass production.
The low-temperature-resistant spodumene flotation collector is used for flotation of spodumene, is favorable for improving the grade and the recovery rate of spodumene concentrate, and reduces fluctuation of flotation indexes caused by changes of latitude and altitude.
Drawings
FIG. 1 is a schematic flow diagram of the spodumene flotation separation in example 1 of the present invention;
FIG. 2 is a schematic flow diagram of the spodumene flotation separation of example 2 of the present invention;
FIG. 3 is a schematic flow chart of the spodumene flotation separation in example 3 of the present invention
Detailed Description
The temperature has a great influence on the conventional collector spodumene dressing, the conventional collector is not dispersed in ore pulp under the condition of low temperature, the flotation froth phenomenon is very poor, the selectivity and the collecting performance of the collector do not play normal effects, the concentrate grade is low, the recovery rate is low, the normal-temperature flotation is generally the flotation at the temperature of more than 20 ℃, and the low-temperature flotation is generally the flotation at the temperature of 14-18 ℃. In the research, oleic acid is an important collector for spodumene flotation, and has the defects of low solubility, low temperature resistance, poor selectivity, hard water resistance, poor dispersibility and large using amount in flotation when being used alone. Tall oil is also a very important low-valent fatty acid collecting agent, carbonate ore is used for floating gangue, the collecting performance of the tall oil is better than that of oleic acid, the low-temperature tolerance can be improved by mixing with the oleic acid, and the two collecting agents are combined to generate a co-adsorption phenomenon, generate interaction with each other and can promote and strengthen the flotation of minerals.
A small amount of anionic synergist or nonionic synergist is added into the collecting agent for compounding, so that compared with the single use or the simple addition effect, the collecting agent can improve the characteristics of the agent, improve the recovery rate, improve the selectivity of the agent and reduce the consumption of the agent. According to the invention, a large number of experimental researches show that the collection performance of oleic acid and tall oil can be enhanced by adding a proper amount of anionic synergist sodium dodecyl benzene sulfonate, the emulsifiers adopt nonionic synergists T-80 and S-80, the nonionic synergists T-80 and S-80 and the nonionic synergists T-80 and S-80 are emulsified by using different HLB (hydrophilic-lipophilic balance) values to the collecting agent, so that the dispersibility and water solubility of the oleic acid and the tall oil can be improved, and the emulsifying effect of the T-80 and S-80 is enhanced by using triethanolamine, so that the emulsifying effect is kept long-acting and is not easy to demulsify. The compounding of the oleic acid, the tall oil and the emulsifier can reduce the addition of the collecting agent by times and improve the recovery rate.
The collecting agent is prepared by mixing and compounding the components, the source of materials is wide, the price is low, the problem of dispersion of the spodumene collecting agent in ore pulp is solved by compounding oleic acid, tall oil and sodium alkyl benzene sulfonate, the collecting agent has good collecting capability and selectivity in low-temperature ore pulp, and the improvement of the grade and the recovery rate of spodumene concentrate is facilitated.
For a better understanding of the present invention, reference will now be made in detail to the present embodiments of the invention, which are illustrated in the accompanying drawings. The reagents used in the examples of the present invention, not specifically described, may be any of commercially available conventional products, and in the following examples, li 2 The content of O is tested according to the GB/T17413.1-2010 standard method; the pulp fineness is measured by a wet screening method through a standard inspection screen; li 2 The O yield is measured by weighing and calculating different products; li 2 O recovery based on Li of product 2 The O grade and the yield are calculated, and the pulp concentration refers to the weight concentration of the ore in the ore and the water.
Example 1
A low-temperature-resistant spodumene flotation collector comprises the following raw materials in parts by weight: preparing C12-18 sodium alkyl benzene sulfonate and emulsifier at a ratio of 57.2: 24.5: 3.9: 14.4; the preparation method comprises the following steps:
A. weighing 57.2 parts of oleic acid, 24.5 parts of crude tall oil and 3.9 parts of sodium dodecyl benzene sulfonate; stirring oleic acid in a water bath at 45 ℃, adding crude tall oil, stirring for 20min, adding 3.9 parts of sodium dodecyl benzene sulfonate in a water bath at 60 ℃, stirring for 20min to completely dissolve the mixture, and fully mixing the mixture;
B. weighing 5.3 parts of T-80 (polyoxyethylene ether sorbitan fatty acid ester), 8.3 parts of S-80 (sorbitan monooleate) and 0.8 part of triethanolamine, mixing, slowly adding into the uniformly mixed materials, and stirring for 40min to obtain brown oily matter, namely the low-temperature-resistant spodumene flotation collector, wherein the stirring rate in A and B is 300r/min.
The prepared flotation collecting agent is adopted to perform flotation separation on spodumene ores, the adopted spodumene raw ores are spodumene ores of a certain selection factory in Yajiang county of Cuminum of Sichuan province, and the spodumene raw ores contain Li 2 1.12 percent of O, associated tantalum-niobium ore, gangue minerals mainly comprising quartz and feldspar, and other minerals such as tourmaline, biotite, chlorite, garnet and the like. The tantalum-niobium minerals are mainly tantalite-niobium-iron-ore homogeneous-phase series minerals.
As shown in fig. 1, the flotation process is performed in a high altitude area in kanzi, the air temperature is low all the year round, in order to reduce the low-temperature flotation environment of a separation plant, the water for flotation supplement in the embodiment adopts ice water with the temperature of 0-4 ℃ frozen by an ice chest, ice bags are hung around a flotation tank in the flotation process, so that the following flotation tests are carried out in the ore pulp environment with the temperature of 10-15 ℃, and the following flotation processes are performed through a closed flotation process in which the flotation is easy to float, spodumene is coarse and coarse, the flotation is fine and one scan, the flotation is easy to float and does not participate in circulation, and middlings are returned sequentially, and the operation is specifically as follows:
(1) Grinding the spodumene raw ore, adding the raw ore and sodium carbonate into the ore grinding machine, wherein the using amount of the sodium carbonate is 1000g/t according to the raw ore, the grinding concentration is 60%, the grinding fineness is-0.074 mm and accounts for 75%, adding ice water to obtain ore pulp, the ore pulp concentration is 45%, and the pH is 8.5;
(2) Adding 30g/t naphthenic acid soap (note: all t below are according to the weight of spodumene raw ore) into the ore pulp obtained in the step (1), stirring for 3min, then performing air flotation, scraping bubbles to obtain easily floating impurities, and obtaining the spodumene ore dressing ore pulp at the bottom of the tank.
(3) Adding a pH regulator sodium hydroxide and an activator calcium chloride into the spodumene ore dressing pulp obtained in the step (2), wherein the using amount of the sodium hydroxide is 1500g/t, the using amount of the calcium chloride is 100g/t, the stirring speed is 2000r/min, stirring is carried out for 30min, the pulp concentration is 45% at the moment, the pH value of the pulp is 12, adding ice water to adjust the pulp concentration to 30% after the stirring is finished, adding the low-temperature-resistant spodumene flotation collector prepared in the example 1 (the using amount of the collector is 600g/t calculated by raw ore, and the collector is added by an aqueous solution with the weight percentage concentration of 5%), carrying out inflation flotation after stirring for 3min, scraping bubbles to obtain spodumene rough flotation foams, and collecting pulp at the bottom of a tank;
(4) Performing blank concentration on the rough concentration foam obtained in the step (3) twice (the blank concentration is to add water without adding any medicament, wherein the concentration of the ore pulp needs to be adjusted to be 15% in the first-stage concentration, air is filled to scrape the foam after stirring for 2min, and the concentration of the ore pulp in the second-stage concentration is 10%), and then fully stirring for 2min for scraping the foam each time to finally obtain a spodumene concentrate product;
(5) Adding 20g/t of calcium chloride according to the raw ore into scavenging ore pulp at the bottom of the tank in the step (3), stirring for 2min, adding the low-temperature-resistant spodumene flotation collecting agent prepared in the example 1 (the using amount of the collecting agent is 120g/t according to the raw ore, the collecting agent is added by using an aqueous solution with the weight percentage concentration of 5%), stirring for 3min, performing air flotation, and taking scraping foam as scavenging foam products and spodumene flotation tailings at the bottom of the tank.
The flotation spodumene results obtained are shown in table 1.
TABLE 1 spodumene closed-loop test results
Example 2
The embodiment provides a low temperature resistant spodumene flotation collector, which comprises the following raw materials in percentage by weight:
oleic acid: crude tall oil: c12-18 sodium alkyl benzene sulfonate and emulsifier are 60: 22.1: 3.5: 14.4; the preparation method comprises the following steps:
A. weighing 60 parts of oleic acid, 22.1 parts of crude tall oil and 3.5 parts of sodium dodecyl benzene sulfonate which are raw materials in parts by weight, stirring the oleic acid under the condition of water bath at 45 ℃, slowly adding the crude tall oil, stirring for 20min, adding 3.5 parts of sodium dodecyl benzene sulfonate under the condition of water bath at 60 ℃, stirring for 20min, completely dissolving the materials, and fully and uniformly mixing;
B. weighing 5.3 parts of T-80 (polyoxyethylene ether sorbitan fatty acid ester), 8.3 parts of S-80 (sorbitan monooleate) and 0.8 part of triethanolamine, mixing, slowly adding into the uniformly mixed materials, and stirring for 30min to obtain brown oily matter, namely the low-temperature-resistant spodumene flotation collector, wherein the stirring rate in A and B is 300r/min.
The prepared flotation collecting agent is adopted to perform flotation separation on spodumene ores, the adopted spodumene raw ores are spodumene ores of Tamarix beaches in Xinjiang and Tian county, the mines are located at an elevation of 5500m and are at a low temperature throughout the year, and the spodumene raw ores contain Li 2 1.43 percent of O, associated tantalum-niobium ore and other minerals mainly comprising quartz, potassium feldspar, albite, lepidolite, biotite, sodalite, muscovite and the like.
The specific flotation process is shown in figure 2, because the temperature of the concentration plant is low throughout the year, in order to reduce the low-temperature flotation environment of the concentration plant, the flotation replenishing water adopts ice water with the temperature of 0-4 ℃ frozen by a freezer, ice bags are hung around the flotation tank in the flotation process, so that the following flotation tests are carried out in the ore pulp environment with the temperature of 10-14 ℃, and the following flotation processes are carried out through a closed flotation process in which one section is easy to float, one rough and two fine scans are carried out on spodumene, the easy flotation does not participate in circulation, and middlings are sequentially returned, and the specific operation is as follows:
(1) Grinding the spodumene raw ore, adding the raw ore and sodium carbonate into the ore grinding machine, wherein the use amount of the sodium carbonate is 1400g/t, the grinding concentration is 60%, the grinding fineness is-0.074 mm and accounts for 70%, adding ice water to adjust the concentration of the ore pulp to 45%, and adjusting the pH value to 8.0;
(2) Adding 35g/t naphthenic acid soap (note: all t below are based on the weight of spodumene raw ore) into the ore pulp obtained in the step (1), stirring for 3min, performing air flotation, scraping bubbles to obtain easily-floating impurities, and obtaining the spodumene ore dressing ore pulp at the bottom of the tank.
(3) Adding a pH regulator sodium hydroxide and an activator calcium chloride into the ore pulp obtained in the step (2), wherein the using amount of the sodium hydroxide is 800g/t calculated according to raw ore, the using amount of the calcium chloride is 80g/t calculated according to raw ore, the ore pulp concentration is 45%, the ore pulp pH value is 12, fully stirring is carried out for 30min, the stirring speed is 2000r/min, ice water is added to adjust the ore pulp concentration to 30% after stirring is finished, adding the prepared low-temperature-resistant spodumene flotation collector (the using amount of the collector is 750g/t calculated according to raw ore, firstly preparing the collector into an aqueous solution with the weight percentage concentration of 5%, then adding the aqueous solution of the collector), carrying out aeration flotation after stirring for 3min, scraping bubbles to obtain spodumene rough flotation foam, and the bottom of a cell is scavenging ore pulp;
(4) Performing blank concentration twice on the rough concentration foam obtained in the step (3) (the blank concentration is that no medicament is added and only water is added, wherein the concentration of ore pulp needs to be adjusted to be 15% in the first-stage concentration, air is filled to scrape bubbles after stirring for 2min, the concentration of ore pulp in the second-stage concentration is 10%), and fully stirring for 2min for scraping bubbles in each concentration, so as to finally obtain a spodumene concentrate product;
(5) Adding 10g/t of calcium chloride according to the raw ore into scavenging ore pulp at the bottom of the tank in the step (3), stirring for 2min, adding the prepared low-temperature-resistant spodumene flotation collecting agent (the using amount of the collecting agent is 100g/t according to the raw ore, and the collecting agent is added in an aqueous solution with the weight percentage concentration of 5%), stirring for 3min, performing air flotation, taking scraping foam as scavenging foam products, and taking spodumene flotation tailings at the bottom of the tank.
The flotation spodumene results as shown in table 2 were obtained.
TABLE 2 spodumene closed-loop test results
Example 3
The embodiment provides a low temperature resistant spodumene flotation collector, which comprises the following raw materials in percentage by weight:
oleic acid: crude tall oil: c12-18 sodium alkyl benzene sulfonate and emulsifier are 56.3: 24.6: 3.3: 15.8; the preparation method comprises the following steps:
A. weighing 56.3 parts of oleic acid, 24.6 parts of crude tall oil and 3.3 parts of sodium dodecyl benzene sulfonate, stirring the oleic acid under the condition of water bath at 45 ℃, adding the crude tall oil, stirring for 20min, adding the sodium dodecyl benzene sulfonate under the condition of water bath at 60 ℃, stirring for 20min to completely dissolve the oleic acid, and fully and uniformly mixing;
B. weighing 5.8 parts of T-80 (polyoxyethylene ether sorbitan fatty acid ester), 9.1 parts of S-80 (sorbitan monooleate) and 0.9 part of triethanolamine, mixing, slowly adding into the uniformly mixed materials, and stirring for 40min to obtain brown oily matter, namely the low-temperature-resistant spodumene flotation collector, wherein the stirring rate in A and B is 300r/min.
The flotation collecting agent prepared by the method is adopted to perform flotation separation on spodumene ores, the adopted spodumene raw ores are Australia imported spodumene ores of a certain selection plant in Tangshan of Hebei, and the raw ores contain Li 2 The O content is 1.63 percent, the spodumene gray white crystal columnar parallel crack distribution and purple and dark brown lepidolite crystals can be seen by naked eyes, the surface has an iron dyeing phenomenon, and the gangue minerals mainly comprise calcium ferrosilicate minerals.
The flotation process is as shown in fig. 3, in order to explore the flotation effect of the collector on the ore in the low-temperature environment, a flotation test in the low-temperature environment is carried out, the flotation replenishing water adopts ice water with the temperature of 0-4 ℃ frozen in an ice chest, ice bags are hung around a flotation tank in the flotation process, so that the following flotation tests are carried out in the ore pulp environment with the temperature of the ore pulp within the range of 14-18 ℃ in the whole process, and the closed flotation process is carried out through one rough and two fine scans of spodumene and the sequential return of middlings, and the specific operation is as follows:
(1) Grinding the spodumene raw ore, adding the raw ore and sodium carbonate into the ore grinding machine, wherein the using amount of the sodium carbonate is 1000g/t, the grinding fineness is-0.074 mm and accounts for 77%, adding ice water, adjusting the concentration of the ore pulp to 45%, and the pH value of the ore pulp is 8.5;
(2) Adding a pH regulator sodium hydroxide and an activator calcium chloride into the ore pulp obtained in the step (1), wherein the using amount of the sodium hydroxide is 800g/t calculated according to raw ore, the using amount of the calcium chloride is 100g/t calculated according to raw ore, fully stirring for 30min at a stirring speed of 2000r/min, the pH value of the ore pulp is 12, after the stirring is finished, adding ice water to regulate the concentration of the ore pulp to 30%, adding the prepared low-temperature-resistant spodumene flotation collector (the using amount of the collector is 550g/t calculated according to raw ore, and the collector is added in an aqueous solution with the weight percentage concentration of 5%), stirring for 3min, performing inflation flotation, scraping bubbles to obtain spodumene rough flotation foam, and collecting ore pulp at the bottom of a scavenging tank;
(3) Performing blank concentration twice on the rough concentration foam obtained in the step (2) (the blank concentration is that no medicament is added and only water is added, wherein the concentration of ore pulp needs to be adjusted to be 15% in the first-stage concentration, air is filled to scrape bubbles after stirring for 2min, the concentration of ore pulp in the second-stage concentration is 10%), and fully stirring for 2min for scraping bubbles in each concentration, so as to finally obtain a spodumene concentrate product;
(4) Adding 30g/t of calcium chloride into the scavenging ore pulp at the bottom of the tank in the step (2), stirring for 2min, adding the prepared low-temperature-resistant spodumene flotation collecting agent (the using amount of the collecting agent is 120g/t based on the raw ore, and the collecting agent is added by using an aqueous solution with the weight percentage concentration of 5%), stirring for 3min, performing air flotation, wherein the froth scraping is a scavenging foam product, and the bottom of the tank is spodumene flotation tailings.
The flotation spodumene results as shown in table 3 were obtained.
TABLE 3 closed-loop test results for spodumene
As can be seen from the flotation indexes in tables 1, 2 and 3, the low temperature resistant spodumene flotation collector disclosed by the invention has good collecting capability and selectivity under a low temperature condition, can obtain spodumene concentrate with high grade and recovery rate, has good adaptability to various spodumene ores in different altitude areas, and can stabilize the flotation indexes of a concentrating mill.
Comparative example 1
Comparative example 1 the weight ratio of the flotation collector is: oxidized paraffin wax soap: tall oil =2, and the amount of collector used was 2.8 times the amount of collector used in example 1 according to the invention, the rest being the same as in example 1. The comparative flotation test results are shown in table 4.
TABLE 4
From the test results in table 4, it can be seen that Li concentrate obtained by flotation using the collector formulated in example 1 of the present invention 2 The indexes of O grade and recovery rate are all superior to those of Li concentrate obtained in comparative example 1 2 The grade and recovery index of O. The reason is that the raw materials react in the heating process to generate the low-temperature-resistant spodumene flotation collector; the collecting agents form a co-adsorption phenomenon to generate an interaction effect, and the addition of the anionic synergist and the nonionic synergist enhances the dispersibility, water solubility and low temperature resistance of the collecting agents, reduces the using amount of the collecting agents and is beneficial to collecting spodumene at low temperature.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. The low-temperature-resistant spodumene flotation collector is characterized by comprising 55-60 parts by weight of oleic acid, 22-28 parts by weight of tall oil, 3-5 parts by weight of sodium alkyl benzene sulfonate and 12-16 parts by weight of an emulsifier.
2. The low temperature resistant spodumene flotation collector of claim 1, wherein the sodium alkyl benzene sulfonate has the general structural formula
Wherein R is a nonpolar group, and R = C12-C18.
3. The low temperature resistant spodumene flotation collector of claim 1, wherein the emulsifier is one or more of polyoxyethylene ether sorbitan fatty acid ester, sorbitan monooleate, and triethanolamine.
4. The low temperature resistant spodumene flotation collector of claim 1, wherein the emulsifier is a mixture of, by weight, 5.3-5.8: 8.3-9.1: 0.8-1 polyoxyethylene ether sorbitan fatty acid ester: sorbitan monooleate: mixtures of triethanolamine.
5. The method for preparing the low temperature resistant spodumene flotation collector of any one of claims 1 to 4, comprising the steps of:
A. heating oleic acid to 40-50 ℃, adding tall oil, stirring, adding sodium alkyl benzene sulfonate under the heating condition of 55-65 ℃, stirring until the sodium alkyl benzene sulfonate is completely dissolved, and fully and uniformly mixing;
B. and adding an emulsifier into the uniformly mixed materials, and continuously stirring to obtain brown oily matter, namely the low-temperature-resistant spodumene flotation collector.
6. The preparation method according to claim 5, wherein in the step A, the time for stirring twice is 20-30 min; and in the step B, continuously stirring for 30-60 min.
7. The application of the low-temperature-resistant spodumene flotation collector in the flotation of spodumene according to any one of claims 1 to 4, wherein the temperature of the added water for flotation is 0-40 ℃, the temperature of flotation pulp is 10-40 ℃, and the dosage of the flotation collector is 400-2000 g/t.
8. A method for flotation of spodumene, characterized in that it comprises the following steps:
s1, grinding spodumene raw ore, wherein the grinding fineness is-200 meshes and accounts for 70-75%, and adding water to obtain ore pulp;
s2, adding a pH regulator and an activator into the ore pulp, regulating the pH to 11-13, mixing the pulp after stirring, adding the flotation collector of any one of claims 1-4 to perform aerated flotation, and scraping bubbles to obtain spodumene rougher flotation foam, wherein the bottom of a tank is scavenging ore pulp;
and S3, carrying out blank concentration on the spodumene rough concentration foam to obtain spodumene concentrate.
9. The method of claim 8, wherein in step S1, sodium carbonate is added to the spodumene raw ore or ore slurry in an amount such that the pH of the ore slurry is adjusted to 8.0 to 8.5, and water is added in an amount such that the mass concentration of the ore slurry is 40 to 45%; adding naphthenic acid soap into the ore pulp, stirring for 2-3 min, aerating, floating to obtain easily floating impurities, and preparing spodumene ore dressing ore pulp at the bottom of the tank;
in the step S2, the pH regulator is sodium hydroxide, and the addition amount of the pH regulator is that the pH value after size mixing is 11-13; the activator is calcium chloride, and the addition amount is 0-150 g/t calculated according to raw ore; the stirring time is 25-35 min, and the stirring speed is 1900-2000 r/min; the adding amount of the flotation collecting agent is 400-2000 g/t calculated by raw ore;
in step S3, the blank selection is to add only water, stir for 2 minutes, and then perform air-filling and foam-scraping.
10. The method of claim 8, further comprising S4, adding the scavenged ore pulp into a flotation collector 30-200 g/t of raw ore, stirring and then performing air flotation, wherein the froth is scraped to form a scavenged foam product, and the bottom of the tank is spodumene flotation tailings.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117443591A (en) * | 2023-10-20 | 2024-01-26 | 广州聚源矿业科技有限公司 | Lithium ore composite collector with high mineralization rate and low foam viscosity and flotation method |
| CN117732599A (en) * | 2024-02-07 | 2024-03-22 | 矿冶科技集团有限公司 | Fatty acid modifier, low temperature resistant spodumene ore medicament, preparation method thereof and method for floating spodumene by using same |
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2022
- 2022-10-31 CN CN202211350899.0A patent/CN115780094A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117443591A (en) * | 2023-10-20 | 2024-01-26 | 广州聚源矿业科技有限公司 | Lithium ore composite collector with high mineralization rate and low foam viscosity and flotation method |
| CN117443591B (en) * | 2023-10-20 | 2024-05-28 | 广州聚源矿业科技有限公司 | Lithium ore composite collector with high mineralization rate and low foam viscosity and flotation method |
| CN117732599A (en) * | 2024-02-07 | 2024-03-22 | 矿冶科技集团有限公司 | Fatty acid modifier, low temperature resistant spodumene ore medicament, preparation method thereof and method for floating spodumene by using same |
| CN117732599B (en) * | 2024-02-07 | 2024-05-31 | 矿冶科技集团有限公司 | Fatty acid modifier, low temperature resistant spodumene ore medicament, preparation method thereof and method for floating spodumene by using same |
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