Preparation method of lepidolite flotation reagent under neutral condition

Abstract

The invention provides a preparation method of a lepidolite flotation reagent under a neutral condition, and relates to the technical field of lepidolite beneficiation. The preparation method of the lepidolite flotation reagent under the neutral condition comprises the following steps that firstly, a proper amount of solvent is added into a reaction container, dodecyl dimethyl tertiary amine and a dispersing agent are added under the condition of magnetic stirring, and magnetic stirring is conducted till the materials are mixed to be uniform for standby application; step 2, continuously adding carboxymethyl cellulose, heating and stirring after adding, and cooling for later use; and thirdly, the foaming agent continues to be added, the high-speed cutting emulsifier is used for emulsification treatment, and the lepidolite flotation reagent is obtained. The lepidolite flotation reagent prepared through the method can be used for lepidolite flotation under the nearly neutral and normal-temperature conditions, corrosion resistance to equipment is small, the obtained lepidolite is high in recovery rate and good in grade, and the lepidolite flotation reagent is suitable for being applied to various lepidolite dressing plants.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of spodumene beneficiation, and particularly relates to a preparation method of a spodumene flotation reagent under neutral conditions. BACKGROUND

[0002] Lithium and its compounds have various industrial applications, and can be used for the production of heat-resistant glass, ceramics, lithium grease lubricant, welding flux additives for iron, steel and aluminum production, lithium batteries and lithium ion batteries, etc. Spodumene, as the most common lithium-containing mineral, is one of the important minerals for refining lithium. Therefore, it is of great significance to improve the development and utilization level of spodumene.

[0003] The content of lithium oxide in different lithium ores is different, and the chemical decomposition process is complex, so the lithium ore separation process is also complex, but the flotation method is used for fine-grained embedded spodumene at home and abroad. Flotation is a method for separating minerals by using the difference between the hydrophobicity and hydrophilicity of the surface of the minerals, and is the most widely used beneficiation method at present. The traditional desliming-acid method or alkali method is a commonly used flotation method, in which the acid flotation process usually uses a single alkyl primary amine as a collector, and spodumene flotation needs to be carried out under strong acidic conditions (pH = 2-4). The strong acid flotation has the problems of poor operation environment, high safety hazard, high requirement for equipment corrosion resistance, serious environmental pollution and difficult wastewater reuse. SUMMARY

[0004] In order to solve the problems of poor operation environment, high safety hazard, high requirement for equipment corrosion resistance, serious environmental pollution and difficult wastewater reuse of the traditional acid flotation process under strong acid conditions, the present application provides a preparation method of a spodumene flotation reagent. The spodumene flotation reagent prepared by the method can be used for spodumene flotation under nearly neutral and normal temperature conditions, has small requirement for equipment corrosion resistance, has high recovery rate of spodumene, has good quality, and is suitable for application in various spodumene beneficiation plants.

[0005] In order to achieve the above-mentioned purpose, the technical scheme adopted by the present application is as follows: a preparation method of a spodumene flotation reagent under neutral conditions, comprising the following steps: Step one, a proper amount of solvent is added to a reaction container, and under the condition of magnetic stirring, dodecyl dimethyl tertiary amine and a dispersing agent are added, and the mixture is stirred magnetically until it is uniformly mixed, and is ready for use; Step two, carboxymethyl cellulose is continuously added, and after the addition is completed, heating and stirring are carried out, and after cooling, it is ready for use; Step three, a foaming agent is continuously added, and emulsification treatment is carried out by using a high-speed cutting emulsifier, to obtain a spodumene flotation reagent.

[0006] In the implementation of the above-mentioned embodiments, preferably, step one is carried out under room temperature conditions.

[0007] In the implementation of the above embodiment, preferably, the stirring speed in step one is 1000-1500 r / min, and the stirring time is 5-10 min.

[0008] In the implementation of the above embodiment, preferably, the heating temperature in step two is 70-85℃.

[0009] In the implementation of the above embodiment, preferably, the stirring speed in step two is 500-800 r / min, and the stirring time is 20-30 min.

[0010] In the implementation of the above embodiment, preferably, the working speed of the high-speed cutting emulsifier in step three is 2000-3000 r / min, and the emulsification time is 10-20 min.

[0011] In the implementation of the above embodiment, preferably, the raw material composition of the lithium mica flotation reagent includes, in mass fraction: 15-20 parts of dodecyl dimethyl tertiary amine, 20-35 parts of carboxymethyl cellulose, 5-8 parts of dispersant, 10-15 parts of foaming agent, and 40-60 parts of solvent.

[0012] In the implementation of the above embodiment, preferably, the foaming agent is selected from one or more of terpineol, carboxyl acid, mixed fatty alcohol, isomeric hexanol or octanol, and ether alcohol.

[0013] In the implementation of the above embodiment, preferably, the dispersant is sodium silicate.

[0014] In the implementation of the above embodiment, preferably, the solvent is water.

[0015] Compared with the prior art, the present application has the following beneficial features: 1. The lithium mica flotation reagent of the present application adds carboxymethyl cellulose in the raw material composition. Carboxymethyl cellulose belongs to organic high polymer material, has large relative molecular mass, and high degree of branching and bending. It not only forms a hydrophilic layer on the surface of gangue minerals, but also covers the hydrophobic layer of the collector on the surface of gangue minerals, so that the gangue minerals are strongly inhibited, and the collection of lithium mica under neutral conditions is realized. In a neutral environment with pH of 6-7, the recovery rate of the collection system of the lithium mica flotation reagent of the present application is increased by more than 20% compared with the recovery rate of the traditional single amine collector on lithium mica.

[0016] 2. The lithium mica flotation reagent of the present application adds sodium silicate in the raw material composition. Sodium silicate has good water solubility, and a specific weight of sodium silicate plays the role of dispersant in the flotation operation, which can effectively disperse the slime. At the same time, carboxymethyl cellulose can be introduced into the interlayer of the lithium ore particle surface under the action of sodium silicate, and the porosity and interlayer spacing of the lithium ore particle are increased, which has obvious effect on improving the grade of lithium mica concentrate.

[0017] 3、The lithium mica flotation reagent of the present application is used for the flotation of lithium mica under nearly neutral and normal temperature conditions, has small corrosion to equipment, has high recovery rate of lithium mica, and has good quality, and is suitable for application in various lithium mica concentrators. DETAILED DESCRIPTION

[0018] To make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described below in a clear and complete manner in conjunction with the embodiments of the present application. Obviously, the described embodiments are some, but not all, of the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present application.

[0019] The reagents used in the examples and comparative examples are described as follows: Dodecyldimethyl tertiary amine: Shandong Jinshun Chemical; Carboxymethyl cellulose: Jinan Sanen Chemical; Dispersant: sodium silicate, Shandong Shuncheng Chemical; Frother: terpineol, Hubei Kovler Chemical; Solvent: water.

[0020] It should be noted that, in the examples, the specific technologies or conditions not specified are performed according to the technologies or conditions described in the literature in the art or according to the product instructions, and the reagents or instruments not specified by the manufacturer are all conventional products that can be obtained from the market. Example 1

[0021] A lithium mica flotation reagent under neutral conditions, in mass parts, includes the following raw material components: 20 parts of dodecyldimethyl tertiary amine, 20 parts of carboxymethyl cellulose, 8 parts of dispersant, 15 parts of frother, and 60 parts of solvent.

[0022] According to the above ratio, the preparation method of the lithium mica flotation reagent under neutral conditions includes the following steps: Step one, 60 parts of solvent are added to a reaction container, and under the condition of magnetic stirring at room temperature, 150 parts of dodecyldimethyl tertiary amine and 8 parts of dispersant are added, and the mixture is stirred uniformly under magnetic stirring at a speed of 1000 r / min for 10 min, and is ready for use; Step two, 20 parts of carboxymethyl cellulose are continuously added, and after the addition is completed, heating is performed to 85℃, and stirring is performed at a stirring speed of 500 r / min for 30 min, and after the stirring is completed, cooling is performed and the mixture is ready for use; Step three, 15 parts of frother are continuously added, and emulsification treatment is performed by using a high-speed cutting emulsifier, the working speed of the high-speed cutting emulsifier is 2000 r / min, the emulsification treatment time is 20 min, and the lithium mica flotation reagent is obtained.

[0023] Flotation test: the Li2O content of the raw ore is 0.6%, the lithium mica raw ore is ground, and then a slurry is prepared by adding water, the pH is adjusted to 6, and then the slurry is poured into a flotation tank for flotation test, and the flotation temperature is 25°C.

[0024] S1: once rough selection, the addition amount of lithium mica flotation reagent is 120g / t, and the rough selection concentrate and rough selection tailings are obtained; S2: once scavenging, the addition amount of lithium mica flotation reagent is 20g / t, and the scavenging concentrate and scavenging tailings are obtained; S3: first selection, the addition amount of lithium mica flotation reagent is 50g / t, and the first selection concentrate and first selection middlings are obtained, and the first selection middlings return to the first rough selection process; S4: second selection, the first selection concentrate is selected without adding lithium mica flotation reagent, and the second selection concentrate and second selection middlings are obtained, and the second selection middlings return to the first selection process. Example 2

[0025] A lithium mica flotation reagent, the raw material composition of which includes, in mass parts: 20 parts of dodecyl dimethyl tertiary amine, 35 parts of carboxymethyl cellulose, 5 parts of dispersant, 10 parts of foaming agent, and 60 parts of solvent.

[0026] According to the above ratio, the preparation steps of the low-temperature lithium mica flotation reagent include the following: Step one, 60 parts of solvent are added to the reaction container, and under the condition of magnetic stirring at room temperature, 120 parts of dodecyl dimethyl tertiary amine and 5 parts of dispersant are added, and the mixture is stirred uniformly, the stirring speed is 1500r / min, the stirring time is 5min, and it is ready for use; Step two, continue to add 35 parts of carboxymethyl cellulose, and after the addition is completed, heat to 70°C, stir, the stirring speed is 800r / min, the stirring time is 20min, after the stirring is completed, cool and prepare for use; Step three, continue to add 10 parts of foaming agent, and emulsify with a high-speed cutting emulsifier, the working speed of the high-speed cutting emulsifier is 3000r / min, the emulsification time is 10min, and the lithium mica flotation reagent is obtained.

[0027] Flotation test: the Li2O content of the raw ore is 0.6%, the lithium mica raw ore is ground, and then a slurry is prepared by adding water, the pH is adjusted to 7, and then the slurry is poured into a flotation tank for flotation test, and the flotation temperature is 25°C.

[0028] S1: once rough selection, the addition amount of lithium mica flotation reagent is 120g / t, and the rough selection concentrate and rough selection tailings are obtained; S2: once the sweep, the sweep of the roughing tailings, the amount of lithium mica flotation reagent is 20g / t, the sweep of the sweep concentrate and tailings; S3: the first selection, the amount of lithium mica flotation reagent is 50g / t, the first selection of the first concentrate and the first selection of the middlings, the first selection of the middlings returns to the first roughing process; S4: the second selection, no lithium mica flotation reagent is added, the first selection of the first concentrate is selected, the second selection of the second concentrate and the second selection of the middlings, the second selection of the middlings returns to the first selection process. Example 3

[0029] A lithium mica flotation reagent, the raw material composition includes: 20 parts of dodecyl dimethyl tertiary amine, 35 parts of carboxymethyl cellulose, 8 parts of dispersing agent, 15 parts of foaming agent and 40 parts of solvent.

[0030] The preparation steps of the low temperature lithium mica flotation reagent according to the above ratio include the following: Step one, 40 parts of solvent are added to the reaction container, and under the condition of magnetic stirring at room temperature, 20 parts of dodecyl dimethyl tertiary amine and dispersing agent are added, and the magnetic stirring is uniform, the magnetic stirring speed is 1500r / min, the stirring time is 10min, and it is ready for use; Step two, continue to add 35 parts of carboxymethyl cellulose, and after adding, heat to 85℃, stir, stirring speed is 800r / min, stirring time is 30min, after stirring, cool and prepare for use; Step three, continue to add 15 parts of foaming agent, and emulsify with high speed cutting emulsifier, the working speed of high speed cutting emulsifier is 3000r / min, the emulsification time is 20min, and the lithium mica flotation reagent is obtained.

[0031] Flotation test: the Li2O content of the raw ore is 0.6%, the lithium mica raw ore is ground and water is added to prepare the ore slurry, the pH value is adjusted to 7, and the flotation test is carried out in the flotation tank, the flotation temperature is 25°C.

[0032] S1: once the roughing, the amount of lithium mica flotation reagent is 120g / t, the roughing concentrate and the roughing tailings are obtained; S2: once the sweep, the sweep of the roughing tailings, the amount of lithium mica flotation reagent is 20g / t, the sweep of the sweep concentrate and tailings; S3: the first selection, the amount of lithium mica flotation reagent is 50g / t, the first selection of the first concentrate and the first selection of the middlings, the first selection of the middlings returns to the first roughing process; S4: the second selection, no lithium mica flotation reagent is added, the first selection of the first concentrate is selected, the second selection of the second concentrate and the second selection of the middlings, the second selection of the middlings returns to the first selection process.

[0033] Comparative Example 1 Commercially available flotation reagents using a single alkyl primary amine as a collector.

[0034] Flotation test: The Li2O content of the raw ore was 0.6%, and the lithium mica raw ore was ground and then made into a slurry with water. The pH was adjusted to 7, and the slurry was poured into a flotation tank for flotation test at a temperature of 25°C.

[0035] S1: once rough selection, the lithium mica flotation reagent was added in an amount of 120 g / t, and a rough selection concentrate and a rough selection tailings were obtained; S2: once scavenging, the lithium mica flotation reagent was added in an amount of 20 g / t, and a scavenging concentrate and a scavenging tailings were obtained; S3: first selection, the lithium mica flotation reagent was added in an amount of 50 g / t, and a first selection concentrate and a first selection middlings were obtained, and the first selection middlings were returned to the once rough selection process; S4: second selection, the lithium mica flotation reagent was not added, and the first selection concentrate was selected to obtain a second selection concentrate and a second selection middlings, and the second selection middlings were returned to the first selection process.

[0036] Comparative Example 2 A lithium mica flotation reagent, in mass parts, includes the following raw material components: dodecyl dimethyl tertiary amine 20 parts, dispersant 5 parts, foaming agent 10 parts, and solvent 60 parts.

[0037] According to the above ratio, the preparation steps of the low-temperature lithium mica flotation reagent include the following: Step one, add an appropriate amount of solvent to the reaction container, and under the condition of magnetic stirring at room temperature, add dodecyl dimethyl tertiary amine and dispersant, and magnetically stir until mixed evenly, the magnetic stirring speed is 1500 r / min, the stirring time is 5 min, and it is ready for use; Step two, continue to add the foaming agent, and emulsify it with a high-speed cutting emulsifier, the working speed of the high-speed cutting emulsifier is 3000 r / min, the emulsification time is 10 min, and the lithium mica flotation reagent is obtained.

[0038] Flotation test: The Li2O content of the raw ore was 0.6%, and the lithium mica raw ore was ground and then made into a slurry with water. The pH was adjusted to 7, and the slurry was poured into a flotation tank for flotation test at a temperature of 25°C.

[0039] S1: once rough selection, the lithium mica flotation reagent was added in an amount of 120 g / t, and a rough selection concentrate and a rough selection tailings were obtained; S2: once scavenging, the lithium mica flotation reagent was added in an amount of 20 g / t, and a scavenging concentrate and a scavenging tailings were obtained; S3: first cleaning, the adding amount of lithium mica flotation reagent is 50 g / t, obtaining cleaning one concentrate and cleaning one middlings, the cleaning one middlings returns the first roughing process; S4: second cleaning, without adding lithium mica flotation reagent, cleaning the cleaning one concentrate, obtaining cleaning two concentrate and cleaning two middlings, the cleaning two middlings returns the first cleaning process.

[0040] Comparative Example 3 A lithium mica flotation reagent, the raw material composition includes, in mass parts: 20 parts of dodecyl dimethyl tertiary amine, 35 parts of carboxymethyl cellulose, 10 parts of foaming agent and 60 parts of solvent.

[0041] According to the above ratio, the preparation steps of the low-temperature lithium mica flotation reagent include the following: Step one, add an appropriate amount of solvent to the reaction container, and under the condition of magnetic stirring at room temperature, add dodecyl dimethyl tertiary amine, and magnetically stir until mixed evenly, the magnetic stirring speed is 1500 r / min, the stirring time is 5 min, and it is ready for use; Step two, continue to add carboxymethyl cellulose, after adding, heat to 70°C, stir, the stirring speed is 800 r / min, the stirring time is 20 min, after stirring, cool and prepare for use; Step three, continue to add the foaming agent, and emulsify it with a high-speed cutting emulsifier, the working speed of the high-speed cutting emulsifier is 3000 r / min, the emulsification time is 10 min, and the lithium mica flotation reagent is obtained.

[0042] Flotation test: the Li2O content of the raw ore is 0.6%, after grinding the lithium mica raw ore, add water to make a slurry, adjust the pH to 7, pour into the flotation tank for flotation test, and the flotation temperature is 25°C.

[0043] S1: once roughing, the adding amount of lithium mica flotation reagent is 120 g / t, obtaining roughing concentrate and roughing tailings; S2: once scavenging, the adding amount of lithium mica flotation reagent is 20 g / t, obtaining scavenging concentrate and scavenging tailings; S3: first cleaning, the adding amount of lithium mica flotation reagent is 50 g / t, obtaining cleaning one concentrate and cleaning one middlings, the cleaning one middlings returns the first roughing process; S4: second cleaning, without adding lithium mica flotation reagent, cleaning the cleaning one concentrate, obtaining cleaning two concentrate and cleaning two middlings, the cleaning two middlings returns the first cleaning process.

[0044] Table 1: flotation results of examples 1-3 and comparative examples 1-3

[0045] The flotation results of examples 1-3 and comparative examples 1-3 are shown in Table 1. From the table, it can be seen that in comparative example 1, using a commercially available flotation agent, the Li2O grade of the lepidolite concentrate is only 1.77% and the recovery rate is 59.65% at pH = 7; in examples 1-3, the Li2O grade of the lepidolite concentrate is more than 4.17% and the recovery rate is more than 81.63%, which is about 20% higher than that of comparative example 1. In comparative example 2, the flotation agent composition lacks carboxymethyl cellulose, which results in a decrease in the Li2O grade and recovery rate of the lepidolite concentrate. In comparative example 3, the flotation agent composition lacks a dispersant, which results in a decrease in the Li2O grade and recovery rate of the lepidolite concentrate.

[0046] It can be seen that the lepidolite flotation agent prepared by the preparation method of the lepidolite flotation agent of the present application can be used for flotation under nearly neutral and normal temperature conditions, the equipment corrosion is small, the recovery rate of the lepidolite obtained is high, the quality is good, and it is suitable for application in various lepidolite concentrators.

[0047] Finally, it should be noted that: the above examples are only used to illustrate the technical solutions of the present application, but not to limit them; although the present application has been described in detail with reference to the above examples, those skilled in the art should understand that: it can still modify the technical solutions recorded in the above examples, or make equivalent replacement for part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for the preparation of a lithium mica flotation reagent under neutral conditions, characterized by, The method comprises the following steps: Step one, add a proper amount of solvent into a reaction container, and under the condition of magnetic stirring, add dodecyl dimethyl tertiary amine and dispersant, and magnetically stir until mixed evenly, and stand by; Step two, continue to add carboxymethyl cellulose, after adding, heat and stir, and after cooling, stand by; Step three, continue to add foaming agent, and emulsify by using high-speed cutting emulsifier, to obtain lithium mica floatation reagent.

2. The method of preparation of lithium mica flotation reagent at neutral conditions according to claim 1, characterized in that, Step one is carried out at room temperature.

3. The method of preparation of lithium mica flotation reagent at neutral conditions according to claim 1, characterized in that, In step one, the stirring speed is 1000-1500 r / min, and the stirring time is 5-10 min.

4. The method of preparing a lithium mica flotation reagent under neutral conditions according to claim 1, characterized in that, In step two, the heating temperature is 70-85℃.

5. The method of preparing a lithium mica flotation reagent under neutral conditions according to claim 1, characterized in that, In step two, the stirring speed is 500-800 r / min, and the stirring time is 20-30 min.

6. The method of preparing a lithium mica flotation reagent under neutral conditions according to claim 1, characterized in that, In step three, the working speed of high-speed cutting emulsifier is 2000-3000 r / min, and the emulsifying time is 10-20 min.

7. The method of preparing a lithium mica flotation reagent at neutral conditions according to claim 1, characterized in that, In terms of mass fraction, the raw material composition of the lithium mica floatation reagent comprises: dodecyl dimethyl tertiary amine 15-20 parts, carboxymethyl cellulose 20-35 parts, dispersant 5-8 parts, foaming agent 10-15 parts, and solvent 40-60 parts.

8. The method of preparation of lithium mica flotation reagent at neutral conditions according to claim 1, characterized by that: The foaming agent is selected from one or more of the following: terpineol, cresylic acid, mixed fatty alcohol, isomeric hexanol or octanol, and ether alcohol.

9. The method of preparation of lithium mica flotation reagent at neutral conditions according to claim 1, characterized by that: The dispersant is sodium silicate.

10. The method of preparing a lithium mica flotation reagent under neutral conditions according to claim 1, characterized by: The solvent is water.

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