Preparation method and application of lithium feldspar collector modification

Abstract

The application belongs to the technical field of collector modification, and particularly relates to a preparation method and application of a modified lithium spodumene collector, which comprises the following steps: taking oxidized paraffin as raw material, placing the oxidized paraffin in an ultraviolet light and electric field environment, connecting an alternating current with a certain frequency to the oxidized paraffin melt under the irradiation of ultraviolet light with a certain wavelength and power, and stirring the reaction for a certain time to obtain a modified lithium spodumene collector product. The lithium spodumene collector prepared by the method has good selectivity, strong collecting capacity, good water solubility and dispersibility, and the raw material required for reaction preparation is easy to obtain, and the reaction process is simple, which has important and positive significance for improving lithium spodumene flotation and improving the efficiency of mineral processing.

Description

Technical Field

[0001] This invention belongs to the field of collector modification technology, specifically relating to a method for preparing modified spodumene collector and its application. Background Technology

[0002] The performance of the collector in flotation directly affects the flotation parameters. The application of high-efficiency spodumene collectors is related to higher lithium concentrate grades and recovery rates, which is of great and positive significance for increasing lithium concentrate production, ensuring the supply of raw materials for the downstream lithium battery industry, and promoting the rapid and healthy development of the new energy industry.

[0003] Currently, one of the main raw materials used in spodumene flotation collectors is oxidized paraffin soap, which is primarily derived from paraffin wax in petroleum products through oxidation and saponification processes. Using oxidized paraffin soap-based fatty acids as a spodumene collector mainly suffers from insufficient selectivity and collection capacity, resulting in a need to improve the recovery rate of lithium concentrate.

[0004] In recent years, mineral processing professionals have primarily focused on mixed collectors in their research on collector compounding techniques using oxidized paraffin soap as a raw material. This includes adding components with stronger selectivity or collecting ability to improve the overall performance of the mixed collector. Research on the synthesis and modification of collectors using oxidized paraffin as a raw material is limited. Therefore, collectors that combine good selectivity, strong collecting ability, and low cost based solely on compounding techniques remain very limited. This is due not only to factors such as the inherently weak selectivity and insufficient collecting ability of the raw materials in compounded collectors, but also, and perhaps more importantly, to a lack of innovative compounding or synthesis techniques, making it difficult to simultaneously achieve a balance between selectivity, collecting ability, and cost. Based on this background analysis, this invention proposes a modified preparation method for a spodumene collector, aiming to innovate the raw material reaction and synthesis process of the collector to form a high-performance spodumene collector for use in the flotation of spodumene ore. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of the prior art and provide a modified preparation method and application of spodumene collector.

[0006] The objective of this invention is achieved through the following technical solution: a method for preparing modified spodumene collector, comprising the following steps: reacting the spodumene collector under ultraviolet light and electric field conditions; The spodumene collector is oxidized paraffin; the ultraviolet light generator used for ultraviolet irradiation has a power of 100W~500W and an ultraviolet light wavelength of 320nm~50nm; the electric field uses alternating current with a frequency of 5~50Hz, a voltage of 10~200V, and an electrode distance of 0.5~5cm; the reaction temperature is 60~120℃, and the reaction time is 2~4 hours.

[0007] Furthermore, the oxidized paraffin is industrial-grade oxidized paraffin.

[0008] Furthermore, the industrial-grade oxidized paraffin has the following composition: 70%~90% oxidized paraffin, 5%~15% paraffin, and 8%~12% alcohol compounds.

[0009] Furthermore, the equipment used in the reaction is a non-conductive reaction vessel, which includes ceramic reaction vessels and glass reaction vessels. The non-conductive reaction vessel is a reactor commonly used in the chemical industry, containing a jacketed oil-heated heating device. There is a jacketed space between the inner and outer walls of the vessel, and heat is conducted through the introduction of circulating and heated oil to bring the reactants to the required temperature.

[0010] Furthermore, the non-conductive reaction vessel is also equipped with a stirrer, an ultraviolet light generator is provided on the top of the inner side of the non-conductive reaction vessel, and an electrode is provided extending upward from the bottom of the non-conductive reaction vessel. The electrode is connected to an alternating current and is located 1 cm away from the rotation range of the stirrer.

[0011] Furthermore, the ultraviolet light generator is an ultraviolet lamp. The stirring speed is 5-60 rpm.

[0012] Furthermore, when using a non-conductive reaction vessel for the modification reaction of oxidized paraffin, the ultraviolet light generator is 20cm to 50cm away from the oxidized paraffin; the height of the immersed electrode is 5 to 10cm lower than the height of the reactants in the reaction vessel.

[0013] Furthermore, the electrodes are arranged uniformly in a matrix, with each pair of adjacent electrodes arranged with positive and negative poles separated and with equal electrode spacing.

[0014] The present invention also provides a modified oxidized paraffin prepared by the above preparation method.

[0015] The present invention also provides an application of the above-mentioned modified oxidized paraffin as a spodumene collector.

[0016] The main innovative aspects of this invention are explained as follows: I. A novel spodumene collector was synthesized by combining ultraviolet light irradiation and an alternating electric field. The reaction principle is as follows: Under ultraviolet light irradiation, oxygen in the air decomposes to produce oxygen free radicals, which have strong chemical reactivity. Under the action of an alternating electric field, the long carbon chain hydrocarbons in oxidized paraffin break down, and the resulting short carbon chain hydrocarbons react with alcohols in the oxidized paraffin under the action of oxygen free radicals to form ethers. The general reaction formula is as follows: R-OH→RO-R'; (R and R' are both hydrocarbon groups, and their carbon chain lengths can be the same or different) Under an alternating electric field, the carboxyl groups in oxidized paraffin exhibit enhanced reactivity, reacting with oxygen free radicals to form the following compounds: R-COOH→R-COOOH The two newly formed compounds, ether and carboxyl peroxide, are favorable for flotation. The ether helps enhance the collector's collecting ability and foaming properties. The carboxyl peroxide significantly enhances the collector's selectivity. The simultaneous presence of both newly formed compounds in the same collector significantly improves the performance of this modified collector.

[0017] Second, the raw material used in the reaction is an industrial-grade raw material, and the components contained in the raw material itself are the source of the reactants, making the raw material source simple and readily available, and the reaction process convenient to operate. The beneficial effects of this invention are: the modified spodumene collector prepared by this invention, due to the improved collector performance caused by the ether groups and peroxide carboxyl groups synthesized through chemical reaction, possesses the characteristics of good selectivity, strong collecting ability, and low cost. Using this modified collector for flotation of spodumene ore can significantly improve concentrate grade and recovery rate. It can be widely applied in the flotation of hard rock spodumene ore both domestically and internationally. Attached Figure Description

[0018] Figure 1 This is a simplified structural diagram of the reaction apparatus used in this invention. Detailed Implementation

[0019] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings, but the scope of protection of the present invention is not limited to the following description.

[0020] See Figure 1 The reaction equipment used in this invention is a ceramic reactor. A stirrer is installed inside the reaction vessel, and an ultraviolet light generator, which is an ultraviolet lamp, is installed on the top of the inner side of the reaction vessel. An electrode with a length of 20 cm is installed extending upward from the bottom of the reaction vessel. The electrode is connected to an alternating current, specifically a controllable frequency alternating current. The electrode is located 1 cm away from the rotation range of the stirrer and is arranged evenly in a matrix. Each pair of adjacent electrodes is arranged with positive and negative poles separated and the electrode spacing is equal.

[0021] Example 1

[0022] A method for preparing a modified spodumene collector, comprising the following steps: (1) Prepare the raw material of oxidized paraffin. Take 100 parts of industrial grade oxidized paraffin raw material. The main components of industrial grade oxidized paraffin raw material are: 82% oxidized paraffin, 10% paraffin, 8% alcohol compounds, etc.

[0023] (2) Using the above-mentioned non-conductive reaction vessel, the distance between adjacent electrodes is set to 1.0 cm, the ultraviolet wavelength is 150 nm, and the power is 500 W.

[0024] (3) Add the prepared paraffin oxide and adjust the distance between the paraffin oxide and the ultraviolet light generator to 20 cm, which is 5 cm higher than the electrode height. Adjust the stirrer speed to 30 rpm, start heating, and the heating rate is 4℃ / min. The reaction temperature is 90℃. Maintain the material temperature after it reaches the set temperature of 90℃.

[0025] (4) Start the ultraviolet light generator, and at the same time start and adjust the frequency of the controllable frequency alternating current to 20Hz and the voltage to 100V, and react for 4 hours.

[0026] (5) After the reaction is complete, turn off the ultraviolet light generator and the electric field power supply, continue stirring for 1 hour, and stop stirring when the temperature of the material in the reactor drops to 50°C. This is the product obtained.

[0027] Experimental Example 1 A comparative example of using the modified oxidized paraffin obtained in Example 1 and the unmodified oxidized paraffin for flotation of spodumene ore.

[0028] The experimental ore was a pegmatite-type spodumene deposit in Aba Prefecture, Sichuan Province. The ore underwent a crushing-grinding process (fineness of -0.074mm and content of 70%) followed by flotation (first-stage roughing). The flotation slurry was adjusted to a pH of 10.5-11.0 using sodium carbonate and sodium hydroxide. The experimental results are shown in Table 1 below. Table 1 Results of comparative tests on collectors

[0029] As shown in Table 1, the modified collector prepared in Example 1 of this invention can significantly improve the grade and recovery rate of Li2O concentrate, and the implementation effect is good.

[0030] Example 2

[0031] A method for preparing a modified spodumene collector, comprising the following steps: (1) Prepare the raw material of oxidized paraffin. Take 100 parts of industrial grade oxidized paraffin raw material. The main components of industrial grade oxidized paraffin raw material are: 75% oxidized paraffin, 13% paraffin, 12% alcohol compounds, etc.

[0032] (2) Using the above-mentioned non-conductive reaction vessel, the distance between adjacent electrodes is set to 2.0 cm, the ultraviolet wavelength is 100 nm, and the power is 400 W.

[0033] (3) Add the prepared paraffin oxide and adjust the distance between the paraffin oxide and the ultraviolet light generator to 30cm, which is 5cm higher than the electrode height. Adjust the stirrer speed to 35 rpm, start heating, and the heating rate is 3℃ / min. The reaction temperature is 100℃. Maintain the material temperature after it reaches the set temperature of 100℃.

[0034] (4) Start the ultraviolet light generator, and at the same time start and adjust the frequency of the controllable frequency alternating current to 30Hz and the voltage to 150V, and react for 3 hours.

[0035] (5) After the reaction is complete, turn off the ultraviolet light generator and electric field power supply, continue stirring for 1.5 hours, and stop stirring when the temperature of the material in the reactor drops to 50°C. This is the product obtained.

[0036] Experimental Example 2 A comparative example of using the modified oxidized paraffin obtained in Example 2 and the unmodified oxidized paraffin for flotation of spodumene ore was presented.

[0037] The experimental ore was a pegmatite-type spodumene deposit in the Pilbara region of Australia. The ore underwent a crushing-grinding process (fineness of -0.074mm and content of 65%)-flotation (first-stage roughing). The flotation slurry was adjusted to a pH of 10.5-11.0 using sodium carbonate and sodium hydroxide. The experimental results are shown in Table 2 below. Table 2 Results of comparative tests on collectors As shown in Table 2, the modified collector prepared in the embodiments of the present invention can improve the grade of Li2O in concentrate and significantly increase the recovery rate, demonstrating good implementation effect.

[0038] The above description is merely a preferred embodiment of the present invention. It should be understood that the present invention is not limited to the forms disclosed herein and should not be construed as excluding other embodiments. It can be used in various other combinations, modifications, and environments, and can be altered within the scope of the concept described herein through the above teachings or related technologies or knowledge. Modifications and variations made by those skilled in the art that do not depart from the spirit and scope of the present invention should be within the protection scope of the appended claims.

Claims

1. A method for preparing a modified spodumene collector, characterized in that, Includes the following steps: The spodumene collector was reacted under ultraviolet light and an electric field. The spodumene collector is oxidized paraffin; the ultraviolet light generator used for ultraviolet irradiation has a power of 100W~500W and an ultraviolet light wavelength of 320nm~50nm; the electric field uses alternating current with a frequency of 5~50Hz, a voltage of 10~200V, and an electrode distance of 0.5~5cm; the reaction temperature is 60~120℃, and the reaction time is 2~4 hours.

2. The method for preparing a modified spodumene collector according to claim 1, characterized in that, The oxidized paraffin is industrial grade oxidized paraffin.

3. The method for preparing a modified spodumene collector according to claim 2, characterized in that, The industrial-grade oxidized paraffin has the following composition: 70%~90% oxidized paraffin, 5%~15% paraffin, and 8%~12% alcohol compounds.

4. The method for preparing a modified spodumene collector according to claim 1, characterized in that, The equipment used for the reaction is a non-conductive reaction vessel, which includes ceramic reaction vessels and glass reaction vessels.

5. The method for preparing a modified spodumene collector according to claim 4, characterized in that, The non-conductive reaction vessel is also equipped with a stirrer, an ultraviolet light generator is installed on the top of the inner side of the non-conductive reaction vessel, and an electrode is installed extending upward from the bottom of the non-conductive reaction vessel. The electrode is connected to an alternating current and is located 1 cm away from the rotation range of the stirrer.

6. The method for preparing a modified spodumene collector according to claim 5, characterized in that, When using a non-conductive reaction vessel for the modification reaction of oxidized paraffin, the ultraviolet light generator is 20cm to 50cm away from the oxidized paraffin; the height of the immersed electrode is 5 to 10cm lower than the height of the reactants in the reaction vessel.

7. The method for preparing a modified spodumene collector according to claim 5, characterized in that, The electrodes are arranged uniformly in a matrix, with each pair of adjacent electrodes arranged with positive and negative poles separated and with equal electrode spacing.

8. Modified oxidized paraffin prepared by the preparation method according to any one of claims 1-7.

9. The application of the modified oxidized paraffin as a spodumene collector according to claim 8.

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