Method for fluorine-free and acid-free flotation separation of feldspar and quartz

By using a specific combination of cationic and anionic collectors, the problems of equipment corrosion and environmental pollution in the separation of feldspar and quartz have been solved, achieving a highly efficient and environmentally friendly fluorine-free and acid-free flotation separation effect.

CN116140070BActive Publication Date: 2025-11-07YICHUN JIANGLI LITHIUM BATTERY NEW ENERGY IND RES INST +2
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Patent Information

Application Number
CN202310171029.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-02-27
Publication Date
2025-11-07
Estimated Expiration
2043-02-27

AI Technical Summary

Technical Problem

Existing methods for separating feldspar and quartz have problems such as easy corrosion of equipment, environmental unfriendliness, and large reagent consumption, especially when flotation separation is carried out in the presence of fluorine and acid.

Method used

A combination of cationic collectors, primarily polyquaternary ammonium salts and mixed amines, and anionic collectors, primarily polyoxyethylene monolaurate, sodium hexadecyl diphenyl ether disulfonate, disodium octadecyl succinate sulfonate, and cottonseed oil soap, is used to achieve fluorine-free and acid-free flotation separation of feldspar and quartz.

Benefits of technology

Efficient separation of feldspar and quartz was achieved without the addition of quartz inhibitors and under fluorine-free and acid-free conditions, resulting in high-purity feldspar concentrate and quartz concentrate. This reduced the amount of reagents used and avoided equipment corrosion and environmental pollution.

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Abstract

The application discloses a fluorine-free and acid-free flotation separation method for feldspar and quartz, and belongs to the technical field of ore dressing. The method comprises the following steps: uniformly mixing polyquaternary ammonium salt 7, polyquaternary ammonium salt 10, polyquaternary ammonium salt 39 and mixed amine in proportion to obtain a cationic collector; uniformly mixing polyoxyethylene monolaurate, sodium cetyl diphenyl ether disulfonate, disodium octadecyl succinate sulfonate and cotton oil acid soap in proportion to obtain an anionic collector; adding lithium mica flotation tailings and water into a flotation machine, adding 50-200 g / t of sodium hexametaphosphate, stirring for 10-20 min, then adding 100-500 g / t of the cationic collector, stirring for 20-30 min, then adding 100-500 g / t of the anionic collector, stirring for 20-30 min, and then carrying out air flotation and bubble scraping to obtain feldspar rough concentrate and quartz rough concentrate; and the method has the characteristics of not corroding equipment, being environment-friendly and being good in feldspar and quartz flotation separation effect.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of mineral processing, and particularly relates to a fluorine-free and acid-free flotation separation method for feldspar and quartz. BACKGROUND

[0002] The main mineral components of typical lithium mica ore in Yichun area are lithium mica, feldspar, quartz, magnetic minerals and the like. After the lithium mica is subjected to desliming, flotation and magnetic separation to remove iron, the tailings of the mineral processing are feldspar and quartz. The tailings of the mineral processing mainly containing feldspar and quartz are difficult to process, and must be efficiently separated to obtain high-purity feldspar and quartz concentrates, so as to improve the product value and thus the product sales and enterprise benefits. Since feldspar and quartz both belong to silicate minerals and have similar floatability, it is difficult to separate feldspar and quartz.

[0003] A method for separating quartz from low-grade potassium-sodium feldspar ore (CN109174434B) crushes, rubs, grinds, deslimes, removes iron, grinds and rubs the low-grade potassium-sodium feldspar ore, adds hydrochloric acid to the obtained rubbing product to adjust the pH value to 2, and then adds sodium carbonate, dodecyl diamine, cetyl polyoxyethylene ether and dodecanol, mixes uniformly, removes the surface foam, and floats out the quartz slurry to obtain a potassium-sodium feldspar concentrate slurry. Although the feldspar-quartz flotation separation effect is good, the slurry needs to be adjusted to pH = 2, and strong acid is easy to corrode the equipment.

[0004] A feldspar-quartz flotation separation combined collector (CN107185721B) is composed of the following raw materials in parts by weight: 1-butylpyridine hydrochloride 2-5 parts, sodium dodecyl sulfonate 2-5 parts, and kerosene 1-3 parts. The total amount of 1-butylpyridine hydrochloride, sodium dodecyl sulfonate and kerosene added is 40-200 g / ton of raw ore. After the slurry concentration is adjusted to 30%-35%, sulfuric acid is added to adjust the slurry pH to 2-5. The feldspar-quartz flotation separation combined collector in an amount of 20-100 g / ton of raw ore is added for coarse feldspar roughing. After the slurry concentration of the coarse feldspar roughing tailings is adjusted to 70%-80%, regrinding is performed, and the grinding degree is adjusted to more than 65% of -0.074 mm. After the regrinding slurry concentration is adjusted to 25%-35%, sulfuric acid is added to adjust the slurry pH to 2-5, then 600-1000 g / ton of raw ore of the adjusting agent acidified water glass is added, and the remaining feldspar-quartz flotation separation combined collector is added for fine feldspar roughing. Although the combined collector has good effect, a large amount of sulfuric acid needs to be added for slurry adjustment, which leads to easy corrosion of the flotation equipment.

[0005] A certain quartz mine cation and anion mixed collector flotation purification research (Yufu Jia, Huang Jie, Chen Xiaolong, etc. A certain quartz mine cation and anion mixed collector flotation purification research [J]. Non-ferrous metal mine, 2015, 38 (5): 57-59.) With a certain quartz mine as raw material, oxalic acid and sodium fluorosilicate as activator, the mixed collector composed of sodium oleate / dodecylamine is used for reverse flotation, and good purification index of SiO2 grade of 99.93% and yield of 62% is obtained. After flotation separation, the removal rate of impurities Al in the ore can reach 99.03%, and the flotation purification effect is obvious. Although the flotation separation effect, the process belongs to fluorine and acid process, which will produce fluorine-containing wastewater.

[0006] In summary, the existing feldspar and quartz are mainly floated and separated in the environment with fluorine and acid, which has problems of easy corrosion of equipment, environmental unfriendliness, large amount of reagent consumption and the like. SUMMARY

[0007] The technical problem to be solved by the present application is to provide a feldspar and quartz fluorine-free and acid-free flotation separation method, which is not easy to corrode equipment, is environmentally friendly, has less reagent consumption, and has good feldspar and quartz flotation separation effect.

[0008] To solve the above technical problems, the present application provides the following technical solutions:

[0009] The method comprises the following steps:

[0010] S1: preparing a cationic collector:

[0011] Polyquaternary ammonium salt 7, polyquaternary ammonium salt 10, polyquaternary ammonium salt 39 and mixed amine are mixed uniformly according to a mass ratio of (0.1-0.2):(0.2-0.4):(0.2-0.4):(0.2-0.4) to obtain a cationic collector;

[0012] S2: preparing an anionic collector:

[0013] Polyoxyethylene monolaurate, sodium hexadecyl diphenyl ether disulfonate, sodium octadecyl succinamide sulfonate, cotton oil acid soap are mixed uniformly according to a mass ratio of (0.1-0.2):(0.2-0.4):(0.2-04):(0.2-0.4) to obtain an anionic collector;

[0014] S3: roughing:

[0015] The lithium mica flotation tailings and water are added into a flotation machine and stirred for 10-20 min;

[0016] Then the cationic collector prepared in step S1 and the anionic collector prepared in step S2 are added, and stirred for 20-30 min;

[0017] Air flotation is carried out to obtain feldspar rough concentrate and flotation tailings;

[0018] (4) Concentration:

[0019] The feldspar rough concentrate obtained in step S3 is subjected to two times of concentration to obtain a feldspar concentrate.

[0020] (5) Scavenging:

[0021] The flotation tailings obtained in step S3 are subjected to two times of scavenging to obtain a quartz concentrate.

[0022] Wherein:

[0023] The polyquaternary ammonium salt 7 in step S1 is dimethyldiallylammonium chloride-acrylamide copolymer, the polyquaternary ammonium salt 10 is chlorinated-2-hydroxy-3-(trimethylammonio) propyl polyethylene oxide cellulose ether, and the polyquaternary ammonium salt 39 is dimethyldiallylammonium chloride-acrylamide-acrylic acid copolymer.

[0024] The mass ratio of the lepidolite flotation tailings and water in step S3 is 1:2.

[0025] The lepidolite flotation tailings in step S3 are tailings obtained after desliming, lepidolite flotation, and magnetic separation of iron from the lepidolite raw ore, and the grade is: K2O+Na2O≥8.0%, Fe2O3≤0.1%, SiO2≥70%.

[0026] The dosage of the cationic collector in step S3 is 10-50 g / t.

[0027] The dosage of the anionic collector in step S3 is 10-50 g / t.

[0028] The first concentration in step S4 is blank concentration, and the second concentration adds 1-5 g / t of the cationic collector prepared in step S1 and 1-5 g / t of the anionic collector prepared in step S2.

[0029] The dosage of the scavenging agent one in step S5 is 1 / 3 of the total dosage of all agents in step S3, and the dosage of the scavenging agent two is 1 / 4 of the total dosage of all agents in step S3.

[0030] Compared with the prior art, the technical scheme of the present application has the following beneficial effects:

[0031] (1) The present invention uses a cationic collector mainly composed of polyquaternary ammonium salt and mixed amine. The multiple quaternary ammonium salt functional groups on the polyquaternary ammonium salt can form binding sites with the Al-O bonds in feldspar, thereby making the feldspar hydrophobic and having strong selectivity. However, it does not act on quartz minerals without metal ion interaction sites, keeping the quartz in a hydrophilic state. Anionic collectors mainly composed of polyoxyethylene monolaurate, sodium hexadecyl diphenyl ether disulfonate, disodium octadecyl succinate sulfonate, and cottonseed oil soap are used. The long carbon chain anionic collector can enhance the hydrophobicity of feldspar after the polyquaternary ammonium salt action, further increasing the difference in floatability between feldspar and quartz, thereby achieving the separation of feldspar and quartz under low dosage conditions.

[0032] (2) The present invention uses cationic quaternary ammonium salt and mixed amine as the main components, and combines them with anionic collectors mainly composed of polyoxyethylene monolaurate, sodium hexadecyl diphenyl ether disulfonate, disodium octadecyl succinate sulfonate and cottonseed oil soap. Since the cationic collector has strong selectivity and the anionic collector has strong hydrophobicity, the combination of the two can achieve efficient separation of feldspar and quartz without adding quartz inhibitors and under fluorine-free and acid-free conditions.

[0033] In summary, this invention can yield feldspar concentrate with a K2O+Na2O grade ≥11%, K2O and Na2O recovery rates ≥90%, and calcination whiteness ≥75%, and quartz concentrate with SiO2 content ≥96%. It overcomes the traditional problem that feldspar and quartz need to be floated under strong acid or fluorine-containing acid conditions. It has the characteristics of not easily corroding equipment, being environmentally friendly, requiring less reagent, and achieving good separation effect of feldspar and quartz flotation. Detailed Implementation

[0034] To make the technical problems, technical solutions and advantages of the present invention clearer, a detailed description will be given below in conjunction with specific embodiments.

[0035] This invention provides a fluorine-free and acid-free flotation separation method for feldspar and quartz.

[0036] The method includes the following steps:

[0037] S1: Preparation of cationic collectors:

[0038] Polyquaternium salt 7, polyquaternium salt 10, polyquaternium salt 39, and mixed amine were mixed evenly in a mass ratio of (0.1-0.2):(0.2-0.4):(0.2-0.4):(0.2-0.4) to obtain a cationic collector.

[0039] S2: Preparation of anion collector:

[0040] Mixing polyoxyethylene monolaurate, sodium cetyl diphenyl ether disulfonate, disodium octadecyl succinamate sulfonate, cotton oil acid soap in a mass ratio of (0.1-0.2):(0.2-0.4):(0.2-0.4):(0.2-0.4) uniformly to obtain an anionic collector;

[0041] S3: rough separation:

[0042] Add the lithium mica flotation tailings and water into the flotation machine and stir for 10-20 min;

[0043] Then add the cationic collector prepared in step S1 and the anionic collector prepared in step S2, and stir for 20-30 min;

[0044] Aerofloat to obtain feldspar rough concentrate and flotation tailings;

[0045] S4: cleaning:

[0046] Carry out two cleaning on the feldspar rough concentrate obtained in step S3 to obtain feldspar concentrate;

[0047] S5: scavenging:

[0048] Carry out two scavenging on the flotation tailings obtained in step S3 to obtain quartz concentrate.

[0049] The following will be described in conjunction with specific examples.

[0050] Example 1

[0051] Take lithium mica flotation tailings as raw material, and the lithium mica flotation tailings are the tailings obtained after desliming, lithium mica flotation, and magnetic separation of iron from the lithium mica raw ore, wherein the specific grade is: K2O+Na2O is 8.5%, Fe2O3 is 0.08%, and SiO2 is 75%.

[0052] Separate feldspar and quartz as follows:

[0053] S1: preparation of cationic collector:

[0054] Mix polyquaternary ammonium salt 7, polyquaternary ammonium salt 10, polyquaternary ammonium salt 39, and mixed amine in a mass ratio of 0.2:0.3:0.3:0.2 uniformly to obtain a cationic collector;

[0055] S2: preparation of anionic collector:

[0056] Mix polyoxyethylene monolaurate, sodium cetyl diphenyl ether disulfonate, disodium octadecyl succinamate sulfonate, and cotton oil acid soap in a mass ratio of 0.2:0.3:0.2:0.3 uniformly to obtain an anionic collector;

[0057] S3: rough separation:

[0058] The lithium mica flotation tailings and water were added into the flotation machine at a mass ratio of 1:2, and stirred for 15 min;

[0059] Then 15 g / t of the cationic collector prepared in step S1 and 20 g / t of the anionic collector prepared in step S2 were added, and stirred for 25 min;

[0060] Air flotation was performed to obtain a feldspar rough concentrate and a flotation tailings;

[0061] S4: cleaning:

[0062] The feldspar rough concentrate obtained in step S3 was subjected to two cleaning operations, wherein the first cleaning was a blank cleaning, and in the second cleaning, 2 g / t of the cationic collector was added, stirred for 15 min, and then 2 g / t of the anionic collector was added, stirred for 12 min, to obtain a feldspar concentrate;

[0063] S5: scavenging:

[0064] The flotation tailings obtained in step S3 were subjected to two scavenging operations, wherein in the first scavenging, 5 g / t of the cationic collector and 6.67 g / t of the anionic collector were added, and stirred for 15 min; and in the second scavenging, 3.75 g / t of the cationic collector and 5 g / t of the anionic collector were added, and stirred for 18 min, to obtain a quartz concentrate.

[0065] In the feldspar concentrate obtained in step S4, the K2O+Na2O grade was 12.5%, the K2O and Na2O recovery rates were 91% and 92% respectively, and the white burning degree was 75%;

[0066] In the quartz concentrate obtained in step S5, the SiO2 content was 96.7%.

[0067] Example 2

[0068] Lithium mica flotation tailings were taken as raw materials. The lithium mica flotation tailings were tailings obtained after desliming, lithium mica flotation, and magnetic separation of iron from the lithium mica flotation tailings. The specific grade was as follows: K2O+Na2O was 8.4%, Fe2O3 was 0.07%, and SiO2 was 74%.

[0069] The feldspar and quartz were separated according to the following steps:

[0070] S1: preparation of a cationic collector:

[0071] The polyquaternary ammonium salt 7, the polyquaternary ammonium salt 10, the polyquaternary ammonium salt 39, and the mixed amine were mixed uniformly at a mass ratio of 0.1:0.3:0.3:0.3 to obtain a cationic collector;

[0072] S2: preparation of an anionic collector:

[0073] Polyoxyethylene monolaurate, sodium cetyl diphenyl ether disulfonate, disodium octadecyl succinimide sulfonate, cotton oil acid soap were mixed uniformly according to the mass ratio of 0.2:0.3:0.2:0.2 to obtain an anionic collector;

[0074] S3: rough separation:

[0075] The lithium mica flotation tailings and water were added into a flotation machine according to the mass ratio of 1:2, and stirred for 12 min;

[0076] Then 20 g / t of the cationic collector prepared in step S1 and 30 g / t of the anionic collector were added, and stirred for 20 min;

[0077] Air flotation was performed to obtain a feldspar rough concentrate and a flotation tailings;

[0078] S4: cleaning:

[0079] The feldspar rough concentrate obtained in step S3 was subjected to two cleaning, wherein the first cleaning was blank cleaning, and in the second cleaning, 3 g / t of the cationic collector was added, stirred for 15 min, and then 2.5 g / t of the anionic collector was added, stirred for 12 min, to obtain a feldspar concentrate;

[0080] S5: scavenging:

[0081] The flotation tailings obtained in step S3 were subjected to two scavenging, wherein in the first scavenging, 6.67 g / t of the cationic collector and 10 g / t of the anionic collector were added, and stirred for 15 min; in the second scavenging, 3.75 g / t of the cationic collector and 7.5 g / t of the anionic collector were added, and stirred for 18 min, to obtain a quartz concentrate.

[0082] In the feldspar concentrate obtained in step S4, the K2O+Na2O grade was 13.5%, the K2O and Na2O recovery rates were 91.6% and 93.1% respectively, and the white burning degree was 76%;

[0083] In the quartz concentrate obtained in step S5, the SiO2 content was 96.9%.

[0084] Example 3

[0085] The lithium mica flotation tailings were taken as raw materials, and the lithium mica flotation tailings were tailings obtained after desliming, lithium mica flotation, and magnetic separation of iron from the lithium mica flotation tailings, wherein the specific grade was: K2O+Na2O was 8.8%, Fe2O3 was 0.05%, and SiO2 was 78%.

[0086] The feldspar and quartz were separated according to the following steps:

[0087] S1: preparation of cationic collector:

[0088] The polyquaternary ammonium salt 7, the polyquaternary ammonium salt 10, the polyquaternary ammonium salt 39, and the mixed amine are mixed uniformly according to a mass ratio of 0.2:0.3:0.3:0.4 to obtain a cationic collector;

[0089] S2: Preparation of an anionic collector:

[0090] The polyoxyethylene monolaurate, the sodium cetyl diphenyl ether disulfonate, the disodium octadecyl succinamate sulfonate, and the cotton oil acid soap are mixed uniformly according to a mass ratio of 0.2:0.3:0.2:0.2 to obtain an anionic collector;

[0091] S3: Roughing:

[0092] The lithium mica flotation tailings and water are added into a flotation machine according to a mass ratio of 1:2, and stirred for 10 min;

[0093] Then, the cationic collector prepared in step S1 is added at 45 g / t, and the anionic collector is added at 30 g / t, and stirred for 20 min;

[0094] Air flotation is performed to obtain a feldspar rough concentrate and a flotation tailings;

[0095] S4: Concentration:

[0096] The feldspar rough concentrate obtained in step S3 is subjected to twice concentration, wherein the first concentration is blank concentration, and in the second concentration, the cationic collector is added at 3.2 g / t, stirred for 15 min, and then the anionic collector is added at 2.8 g / t, stirred for 12 min, to obtain a feldspar concentrate;

[0097] S5: Scavenging:

[0098] The flotation tailings obtained in step S3 are subjected to twice scavenging, wherein in the first scavenging, the cationic collector is added at 15 g / t and the anionic collector is added at 10 g / t, and stirred for 15 min; and in the second scavenging, the cationic collector is added at 11.3 g / t and the anionic collector is added at 7.5 g / t, and stirred for 18 min, to obtain a quartz concentrate.

[0099] In the feldspar concentrate obtained in step S4, the K2O+Na2O grade is 13.5%, the K2O and Na2O recovery rates are 92.3% and 92.8% respectively, and the white burning degree is 76.8%;

[0100] In the quartz concentrate obtained in step S5, the SiO2 content is 97.1%.

[0101] The above is a preferred embodiment of the present application. It should be noted that those skilled in the art can make several improvements and refinements without departing from the principles of the present application, and these improvements and refinements should also be considered within the scope of protection of the present application.

Claims

1. A method for fluorine-free and acid-free flotation separation of feldspar from quartz, characterized by, The steps include the following: S1: preparing cationic collector: Mixing polyquaternary ammonium salt 7, polyquaternary ammonium salt 10, polyquaternary ammonium salt 39 and mixed amine in a mass ratio of (0.1-0.2):(0.2-0.4):(0.2-0.4):(0.2-0.4) uniformly to obtain a cationic collector; S2: preparing anionic collector: Mixing polyoxyethylene monolaurate, sodium cetyl diphenyl ether disulfonate, disodium octadecyl succinamate sulfonate and cotton oil acid soap in a mass ratio of (0.1-0.2):(0.2-0.4):(0.2-0.4):(0.2-0.4) uniformly to obtain an anionic collector; S3: roughing: Adding lithium mica flotation tailings and water into a flotation machine and stirring for 10-20 min; Then adding the cationic collector prepared in step S1 and the anionic collector prepared in step S2 at the same time, stirring for 20-30 min; aerating and floating to obtain feldspar rough concentrate and flotation tailings; S4: cleaning: Carrying out twice cleaning on the feldspar rough concentrate obtained in step S3 to obtain feldspar concentrate; S5: scavenging: Carrying out twice scavenging on the flotation tailings obtained in step S3 to obtain quartz concentrate.

2. The method for fluorine-free and acid-free flotation separation of feldspar from quartz according to claim 1, characterized in that, The polyquaternary ammonium salt 7 in step S1 is dimethyl diallyl ammonium chloride-acrylamide copolymer, the polyquaternary ammonium salt 10 is chlorinated-2-hydroxy-3-(trimethylammonium) propyl polyethylene oxide cellulose ether, and the polyquaternary ammonium salt 39 is dimethyl diallyl ammonium chloride-acrylamide-acrylic acid copolymer.

3. The method for fluorine-free and acid-free flotation separation of feldspar from quartz according to claim 1, characterized in that, The mass ratio of lithium mica flotation tailings to water in step S3 is 1:

2.

4. The method for fluorine-free and acid-free flotation separation of feldspar from quartz according to claim 1, characterized in that, The lithium mica flotation tailings in step S3 are tailings obtained after desliming, lithium mica flotation and magnetic separation of iron from lithium mica raw ore, and the grade is: K2O+Na2O≥8.0%, Fe2O3≤0.1%, SiO2≥70%.

5. The method for fluorine-free and acid-free flotation separation of feldspar from quartz according to claim 1, characterized in that, The dosage of the cationic collector in step S3 is 10-50 g / t.

6. The method for fluorine-free and acid-free flotation separation of feldspar from quartz according to claim 1, characterized in that, The dosage of the anionic collector in step S3 is 10-50 g / t.

7. The method for fluorine-free and acid-free flotation separation of feldspar from quartz according to claim 1, characterized in that, The first cleaning in step S4 is blank cleaning, and the second cleaning adds 1-5 g / t of the cationic collector prepared in step S1 and 1-5 g / t of the anionic collector prepared in step S2.

8. The method for fluorine-free and acid-free flotation separation of feldspar from quartz according to claim 1, characterized in that, The dosage of the scavenging agent in step S5 is 1 / 3 of the total dosage of all agents in step S3, and the dosage of the scavenging agent in step S5 is 1 / 4 of the total dosage of all agents in step S3.

Citation Information

Patent Citations

  • A combined collector for feldspar-quartz flotation separation and its application method

    CN107185721B

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    CN109174434B

  • Efficient combined collector for spodumene and preparation method and application thereof

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    CN112474063A