Feldspar-quartz flotation combined collector and application method thereof

Abstract

The invention discloses a feldspar-quartz flotation combined collecting agent and an application method, and belongs to the technical field of quartz sand processing, the feldspar-quartz flotation combined collecting agent comprises the following components by weight: 1-2 parts of dodecyl trimethyl ammonium chloride, 1.5-3 parts of fatty acid salt, 1-2 parts of a nonionic surfactant, and 1 part of an inhibitor. The dodecyl trimethyl ammonium chloride has good flotation collecting performance, and active Al < 3 + > on the surface of the feldspar is chelated with linoleate ions and adsorbed on the surface of the feldspar. A sodium sulfate inhibitor in a flotation system reduces interfacial tension, the flotation rate of associated impurity minerals is increased, and feldspar and quartz are efficiently separated. The invention further provides the feldspar-quartz flotation combined collecting agent. The method is simple in technological condition, few in operation step, high in purification efficiency, high in safety and feasibility and capable of separating feldspar and quartz in a targeted mode.

Description

Technical Field

[0001] The invention relates to the technical field of quartz sand processing, and in particular to a feldspar-quartz flotation combination reagent and an application method thereof. Background Art

[0002] Quartz is a type of silicate mineral with the characteristics of high hardness, high temperature resistance, and stable physical and chemical properties. High-purity quartz sand refers to quartz sand with a SiO2 content higher than 99.9%. It is mostly prepared by purification or chemical synthesis, and can be used in high-tech industries such as semiconductors, photovoltaics, and optical communications by preparing intermediate products such as quartz crucibles and quartz sleeves. Among them, quartz for semiconductors has the highest requirements for material quality, and the purity must reach 5N or above (>99.999%). At present, the difficulty in preparing high-purity quartz sand lies in the fact that the impurity minerals that grow on the surface of quartz minerals are difficult to remove, especially feldspar in granite pegmatite salt. Feldspar and quartz have similar structures and physical and chemical properties and are not easy to separate. Therefore, how to separate feldspar and quartz to achieve the purification of high-purity quartz sand is a research focus.

[0003] The flotation process can efficiently separate feldspar and quartz. By selecting appropriate flotation reagents, adjusting the ratio of combined reagents, and changing the pH conditions and concentration of the slurry, the purpose of improving flotation efficiency, separating feldspar and quartz, and reducing quartz loss can be achieved. Commonly used flotation separation methods for feldspar and quartz include: fluorine and acid, fluorine-free and acid, and fluorine-free and acid-free methods. The first two require the addition of hydrofluoric acid during the flotation process, which is dangerous to operate and also destructive to equipment and the environment. After this improvement, it is selected to achieve efficient separation of feldspar and quartz under fluorine-free and acid-free conditions in a neutral or weakly alkaline medium, which simplifies the flotation process and reduces production costs.

[0004] The Chinese patent document with publication number CN116140070 A discloses a fluorine-free and acid-free flotation separation method for feldspar and quartz. The invention mixes polyquaternium salt 7, polyquaternium salt 10, polyquaternium salt 39 and mixed amine in proportion to obtain a cationic collector. Polyoxyethylene monolaurate, sodium hexadecyl diphenyl ether disulfonate, disodium octadecyl succinamide sulfonate and cotton oil soap are mixed in proportion to obtain an anionic collector. Sodium hexametaphosphate, cationic collector and anionic collector are added to the slurry prepared from the ore sample and water, stirred, aerated flotation, and scraped to obtain a rough concentrate of feldspar and a rough concentrate of quartz.

[0005] The Chinese patent document with publication number CN107185721A discloses a feldspar-quartz flotation separation combined collector and an application method. The separation combined collector comprises the following components by weight: 2-5 parts of 1-butylpyridine hydrochloride, 2-5 parts of sodium petroleum sulfonate, and 1-3 parts of kerosene. In the feldspar-quartz flotation process, the sand product is first obtained according to the steps of desludging the raw ore, grinding the sand product, magnetic separation, and desludging the non-magnetic product. Then, the feldspar-quartz flotation separation combined collector is added to perform rough selection and selection of coarse-grained feldspar to obtain feldspar concentrate and feldspar flotation tailings. Finally, the feldspar flotation tailings are sedimented and desludged to obtain quartz concentrate.

[0006] In summary, although the above-mentioned existing patents can achieve the separation of feldspar and quartz, the raw materials and proportions of the combined reagents are complex, the process steps are cumbersome, and the impurity removal and separation efficiency are low. In order to improve the above shortcomings and improve the efficiency, the present invention adopts a fluorine-free and acid-free flotation method to separate feldspar and quartz. The reagent composition is simple, the raw materials are easily available, it is safe and environmentally friendly, and it has high feasibility. It has important guiding significance and promotion value for improving the separation and impurity removal efficiency of each flotation operation. Summary of the invention

[0007] The invention discloses a feldspar-quartz flotation combined collector, the components of which are dodecyl trimethyl ammonium chloride, fatty acid salt, nonionic surfactant, and inhibitor, and the flotation separation effect is significantly improved by the synergistic effect of the reagent components. The invention also provides an application method for feldspar-quartz flotation separation, the method has simple operation steps, high ore particle attachment rate and flotation efficiency, excellent safety, and under the premise of ensuring efficient separation of feldspar and quartz, a high-purity quartz product is obtained with less residual impurity elements.

[0008] The specific technical solutions adopted are as follows:

[0009] A feldspar-quartz flotation combined collector comprises the following components in parts by weight: 1-2 parts of dodecyltrimethylammonium chloride, 1.5-3 parts of fatty acid salt, 1-2 parts of nonionic surfactant and 1 part of inhibitor.

[0010] The feldspar-quartz flotation combined collector of the present invention is composed of dodecyl trimethyl ammonium chloride, fatty acid salt, nonionic surfactant and inhibitor in a specific ratio, with simple raw materials and good flotation effect. Dodecyl trimethyl ammonium chloride as a cationic collector has higher flotation selectivity and higher concentrate index, can ensure that the foam viscosity generated during the flotation process is moderate, and has excellent flotation performance. The acid radical ions in the fatty acid salt react with the active Al in the micro-region on the surface of the feldspar. 3+ Combine and react chemically, strongly adsorb on the surface, which is conducive to the separation of quartz and feldspar. In addition, adding an appropriate amount of inhibitor can reduce the solid-liquid interfacial tension, reduce the stickiness of the flotation foam in the ore pulp, and increase the floatation rate of associated impurity minerals, thus achieving the purpose of efficient separation.

[0011] Preferably, the fatty acid salt is at least one of oxidized paraffin soap, sodium linoleate, and sodium petroleum sulfonate.

[0012] Preferably, the nonionic surfactant is at least one of polyethylene glycol monoethyl ether and decapolyoxyethylene ethyl ether, in order to reduce the unfavorable conditions of foaming and stickiness and poor flotation selectivity caused by the action of mineral slime.

[0013] Preferably, the inhibitor is at least one of sodium hexametaphosphate, sodium silicate and sodium sulfate, which is intended to form a hydrophilic film on the surface of the mineral, weaken the adsorption activity of the combined collector, and improve the separation efficiency.

[0014] The present invention also provides an application method of a feldspar-quartz flotation combination reagent, and the flotation process is as follows:

[0015] (1) Weigh dodecyltrimethylammonium chloride, fatty acid salt, nonionic surfactant, inhibitor combined collector raw materials according to proportion, and completely dissolve them in deionized water at a mass ratio of 1:2-6 to prepare a feldspar-quartz flotation combined collector.

[0016] (2) crushing and grinding the feldspar and quartz associated ore, adding deionized water, stirring them fully and settling them to prepare a first slurry.

[0017] (3) Desliming the first slurry and adjusting the slurry concentration to obtain a second slurry. Then, a pH regulator and the feldspar-quartz flotation combined collector prepared in step (1) are added in sequence, stirred, and aerated flotation is performed to separate the quartz from the feldspar.

[0018] (4) Repeat the above step (3), and after secondary flotation, the foam product obtained is quartz, and the residual product in the flotation tank is feldspar.

[0019] Preferably, the fineness of the feldspar quartz associated ore after crushing and grinding is distributed in the range of 0.075-0.145 mm.

[0020] Preferably, the mass concentration of the first slurry is 30-45%, the stirring time is 5-10 minutes, and the sedimentation time is 10 minutes.

[0021] Preferably, the mass concentration of the second slurry is 50-60%, the pH is adjusted to 9-11, 100-200g of feldspar-quartz flotation combined collector is added per ton of raw ore, stirred, and aerated flotation is performed once to separate feldspar and quartz from the associated ore.

[0022] Preferably, the pH is readjusted to 10-11, 50-100 g of feldspar-quartz flotation combined collector is added per ton of raw ore, stirred, and aerated flotation is performed twice to obtain feldspar and quartz products.

[0023] Preferably, the total content of K2O and Na2O in the feldspar product obtained by the feldspar-quartz flotation separation method of the present invention reaches 12.89%, the SiO2 content in the quartz product is ≥99.95%, and a large amount of impurity elements such as Al, Ca, Mg, Fe, Cu, Ni, and Ti are removed.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] (1) The dodecyl trimethyl ammonium chloride in the present invention has better flotation selectivity as a low-chain quaternary ammonium salt, and can combine with acid radical ions to make the active Al 3+ More is adsorbed and co-adsorbed with amine cations, thereby improving the efficiency of the combined collector and improving the flotation effect of feldspar-quartz. Under the action of fatty acid salts, the negative charge of the feldspar surface increases, and the charge of the quartz surface does not change significantly, further expanding the surface potential difference between feldspar and quartz, and improving the collection capacity and selectivity of feldspar. In addition, the inhibitor is used to specifically desorb and cover the collector adsorbed on the quartz surface, thereby inhibiting the flotation of the mineral and achieving the purpose of feldspar-quartz flotation separation.

[0026] (2) The flotation experiment conditions in the present invention are fluorine-free and acid-free, which causes less corrosion to the equipment and environmental damage. At the same time, the raw materials are easily available, the composition is simple, and the operation is convenient. The feldspar-quartz flotation separation method of the present invention can greatly improve the recovery efficiency of feldspar and quartz. DETAILED DESCRIPTION

[0027] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] The present invention will be further described below in conjunction with specific implementation modes.

[0029] Example 1

[0030] In this embodiment, the feldspar-quartz flotation combination reagent is composed of 1 part of dodecyltrimethylammonium chloride, 1.5 parts of sodium linoleate, 1 part of polyethylene glycol monoethyl ether, and 1 part of sodium sulfate, calculated by weight.

[0031] This example uses a potassium-sodium feldspar-quartz associated ore produced in Hunan, and the particle size after crushing and grinding is 0.125-0.21mm, and illustrates the method of flotation using the feldspar-quartz flotation combined collector:

[0032] (1) Take 5 g of dodecyltrimethylammonium chloride, 7.5 g of sodium linoleate, 5 g of polyethylene glycol monoethyl ether, and 5 g of sodium sulfate in a beaker, add 70 mL of deionized water, and stir until completely dissolved to prepare an aqueous solution for use;

[0033] (2) The feldspar-quartz flotation combined collector aqueous solution is used to carry out a coarse and fine flotation of the feldspar quartz associated ore sample. The process conditions and steps are as follows:

[0034] The impeller rotation speed is 1500rpm and the air blowing speed is 0.6m 3 / h. 100 kg of associated ore sample is added to the flotation tank, and deionized water is added to prepare a slurry with a mass concentration of 40%. After stirring for 5 minutes, the first slurry is obtained by settling for 10 minutes, and the slurry is deslimed and the slurry concentration is readjusted to 50% to obtain a second slurry. Then, sodium hydroxide is added to adjust the pH to 9, and the feldspar-quartz flotation combined collector prepared in step (1) (100 g of feldspar-quartz flotation combined collector is added per ton of raw ore) is stirred and aerated for flotation to separate the quartz from the feldspar.

[0035] (3) Repeat the above flotation step (2), adjust the pH to 10, add 80g of feldspar-quartz flotation combined collector per ton of raw ore, stir, and after secondary flotation, the foam product obtained is quartz, and the residual product in the flotation tank is feldspar. ICP-OES is used to detect the chemical composition of the products floating and remaining in the flotation tank.

[0036] Comparative Example 1

[0037] The feldspar-quartz flotation combined collector in Comparative Example 1 is the same as the feldspar-quartz flotation separation collector in Example 1, except that the components do not include dodecylamine trimethylammonium chloride. The combined reagent aqueous solution is prepared using 7.5 g of sodium linoleate, 5 g of polyethylene glycol monoethyl ether, 5 g of sodium sulfate and 70 mL of deionized water;

[0038] The associated ore sample (the same as that in Example 1) was subjected to feldspar-quartz flotation using the feldspar-quartz flotation combination collector in Comparative Example 1 according to the same steps as in Example 1 to obtain feldspar products and quartz products, and the chemical compositions of the products that floated and remained in the flotation cell were characterized.

[0039] ICP-OES was used to detect the chemical composition of feldspar quartz associated ore, Example 1 and Comparative Example 1, and the test results are shown in Table 1. The total content of K2O and Na2O in the feldspar product obtained in Example 1 was 12.89%, and the total content of K2O and Na2O in the feldspar product obtained in Comparative Example 1 was 9.09%. According to the standard chemical ratio of potassium feldspar and sodium feldspar, the SiO2 content in the feldspar products of Example 1 and Comparative Example 1 was 68.85% and 69.04%, respectively.

[0040] Table 1 Comparison of chemical composition of feldspar quartz associated ore, Example 1 and Comparative Example 1 (wt.%)

[0041]

[0042] Example 2

[0043] In this embodiment, the feldspar-quartz flotation combined collector is composed of 1 part of dodecyltrimethylammonium chloride, 1.5 parts of sodium linoleate, 1 part of polyethylene glycol monoethyl ether, and 1 part of sodium sulfate, calculated by weight.

[0044] This example uses potassium-sodium feldspar ore from Hunan, and quartz sand with a particle size of 0.125-0.21 mm after crushing and grinding as raw materials, and illustrates the method of flotation using the feldspar-quartz flotation separation combined reagent:

[0045] This example uses a potassium-sodium feldspar-quartz associated ore produced in Hunan, and the particle size after crushing and grinding is 0.125-0.21mm, and illustrates the method of flotation using the feldspar-quartz flotation combined collector:

[0046] (1) Take 5 g of dodecyltrimethylammonium chloride, 7.5 g of sodium linoleate, 5 g of polyethylene glycol monoethyl ether, and 5 g of sodium sulfate in a beaker, add 100 mL of deionized water, and stir until completely dissolved to prepare an aqueous solution for use;

[0047] (2) The feldspar-quartz flotation combined collector aqueous solution is used to carry out a coarse and fine flotation of the feldspar quartz associated ore sample. The process conditions and steps are as follows:

[0048] The impeller rotation speed is 1500rpm and the air blowing speed is 0.6m 3 / h. 100 kg of associated ore sample is added to the flotation tank, and deionized water is added to prepare a slurry with a mass concentration of 45%. After stirring for 5 minutes, the first slurry is obtained by settling for 10 minutes, and the slurry is deslimed and the slurry concentration is readjusted to 60% to obtain a second slurry. Then, sodium hydroxide is added to adjust the pH to 10, and the feldspar-quartz flotation combined collector prepared in step (1) (150 g of feldspar-quartz flotation combined collector is added per ton of raw ore) is stirred and aerated for flotation to separate the quartz from the feldspar.

[0049] (3) Repeat the above flotation step (2), adjust the pH to 11, add 100g of feldspar-quartz flotation combined collector per ton of raw ore, stir, and after secondary flotation, the foam product obtained is quartz, and the residual product in the flotation tank is feldspar. ICP-OES is used to detect the chemical composition of the products floating and remaining in the flotation tank.

[0050] Comparative Example 2

[0051] The feldspar-quartz flotation combined collector in Comparative Example 1 is different from the feldspar-quartz flotation separation collector in Example 1, except that sodium linoleate is not included in the components. The combined reagent aqueous solution is prepared with 5g of dodecylamine trimethylammonium chloride, 5g of polyethylene glycol monoethyl ether, 5g of sodium sulfate and 100mL of deionized water;

[0052] The associated ore sample (the same as Example 2) was subjected to feldspar-quartz flotation by using the feldspar-quartz flotation combination collector in Comparative Example 2 according to the same steps as Example 2 to obtain feldspar products and quartz products, and the chemical compositions of the products that floated and remained in the flotation cell were characterized.

[0053] ICP-OES was used to detect the chemical composition of feldspar quartz associated ore, Example 2 and Comparative Example 2, and the test results are shown in Table 2. The total content of K2O and Na2O in the feldspar product obtained in Example 2 was 11.85%, and the total content of K2O and Na2O in the feldspar product obtained in Comparative Example 2 was 8.59%. According to the standard chemical ratio of potassium feldspar and sodium feldspar, the SiO2 content in the feldspar products of Example 2 and Comparative Example 2 was 67.35% and 68.27%, respectively.

[0054] Table 2 Comparison of chemical composition of feldspar quartz associated ore, Example 2 and Comparative Example 2 (wt.%)

[0055]

[0056] Example 3

[0057] In this embodiment, the feldspar-quartz flotation combined collector is composed of 1 part of dodecyltrimethylammonium chloride, 1.5 parts of sodium linoleate, 1 part of polyethylene glycol monoethyl ether, and 1 part of sodium sulfate, calculated by weight.

[0058] This example uses potassium-sodium feldspar ore from Hunan, and quartz sand with a particle size of 0.125-0.21 mm after crushing and grinding as raw materials, and illustrates the method of flotation using the feldspar-quartz flotation separation combined reagent:

[0059] (1) Take 5 g of dodecyltrimethylammonium chloride, 7.5 g of sodium linoleate, 5 g of polyethylene glycol monoethyl ether, and 5 g of sodium sulfate in a beaker, add 100 mL of deionized water, and stir until completely dissolved to prepare an aqueous solution for use;

[0060] (2) The feldspar-quartz flotation combined collector aqueous solution is used to carry out a coarse and fine flotation of the feldspar quartz associated ore sample. The process conditions and steps are as follows:

[0061] The impeller rotation speed is 1500rpm and the air blowing speed is 0.6m 3 / h. 100 kg of associated ore sample is added to the flotation tank, and deionized water is added to prepare a slurry with a mass concentration of 40%. After stirring for 8 minutes, the first slurry is obtained by settling for 10 minutes, and the slurry is deslimed and the slurry concentration is readjusted to 55% to obtain a second slurry. Then, sodium hydroxide is added to adjust the pH to 9, and the feldspar-quartz flotation combined collector prepared in step (1) (120 g of feldspar-quartz flotation combined collector is added per ton of raw ore) is stirred, and aerated flotation is performed to separate the quartz from the feldspar.

[0062] (3) Repeat the above flotation step (2), adjust the pH to 10, add 80g of feldspar-quartz flotation combined collector per ton of raw ore, stir, and after secondary flotation, the foam product obtained is quartz, and the residual product in the flotation tank is feldspar. ICP-OES is used to detect the chemical composition of the products floating and remaining in the flotation tank.

[0063] Comparative Example 3

[0064] The feldspar-quartz flotation combined collector in Comparative Example 3 is different from the feldspar-quartz flotation separation collector in Example 3, and the only difference is that the proportion of polyethylene glycol monoethyl ether in the components is different. The combined agent aqueous solution is prepared with 5g of dodecyltrimethylammonium chloride, 7.5g of sodium linoleate, 10g of polyethylene glycol monoethyl ether, 5g of sodium sulfate and 100mL of deionized water;

[0065] The associated ore sample (the same as that in Example 3) was subjected to feldspar-quartz flotation using the feldspar-quartz flotation combination collector in Comparative Example 3 according to the same steps as in Example 3 to obtain feldspar products and quartz products, and the chemical compositions of the products that floated and remained in the flotation cell were characterized.

[0066] ICP-OES was used to detect the chemical composition of feldspar quartz associated ore, Example 3 and Comparative Example 3, and the test results are shown in Table 3. The total content of K2O and Na2O in the feldspar product obtained in Example 3 was 10.84%, and the total content of K2O and Na2O in the feldspar product obtained in Comparative Example 3 was 8.66%. According to the standard chemical ratio of potassium feldspar and sodium feldspar, the SiO2 content in the feldspar products of Example 3 and Comparative Example 3 was 67.68% and 66.34%, respectively.

[0067] Table 3 Comparison of chemical composition of feldspar quartz associated ore, Example 3 and Comparative Example 3 (wt.%)

[0068]

[0069] The embodiments described above provide a detailed description of the technical solutions of the present invention. It should be understood that the above are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, supplements or similar substitutions made within the scope of the principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A feldspar-quartz flotation combined collector, characterized in that: The composition comprises the following components in parts by weight: 1-2 parts of dodecyltrimethylammonium chloride, 1.5-3 parts of fatty acid salt, 1-2 parts of nonionic surfactant and 1 part of inhibitor.

2. The feldspar-quartz flotation combined collector according to claim 1, characterized in that: The fatty acid salt is at least one of oxidized paraffin soap, sodium linoleate and sodium petroleum sulfonate.

3. The feldspar-quartz flotation combined collector according to claim 1, characterized in that: The nonionic surfactant is at least one of polyethylene glycol monoethyl ether and decapolyoxyethylene ethyl ether.

4. The feldspar-quartz flotation combined collector according to claim 1, characterized in that: The inhibitor is at least one of sodium hexametaphosphate, sodium silicate and sodium sulfate.

5. An application method of feldspar-quartz flotation separation, characterized in that: Utilize the feldspar-quartz flotation combined collector described in any one of claims 1-4.

6. The application method of feldspar-quartz flotation separation according to claim 5, characterized in that: The following steps are involved: (1) Weigh dodecyltrimethylammonium chloride, fatty acid salt, nonionic surfactant, inhibitor combined collector raw materials according to proportion, and completely dissolve them in deionized water at a mass ratio of 1:2-6 to prepare a feldspar-quartz flotation combined collector. (2) crushing and grinding the feldspar and quartz associated ore, adding deionized water, stirring them fully and settling them to prepare a first slurry. (3) Desliming the first slurry and adjusting the slurry concentration to obtain a second slurry. Then, a pH regulator and the feldspar-quartz flotation combined collector prepared in step (1) are added in sequence, stirred, and aerated flotation is performed to separate the quartz from the feldspar. (4) Repeat the above step (3), and after secondary flotation, the foam product obtained is quartz, and the residual product in the flotation tank is feldspar.

7. The application method of feldspar-quartz flotation separation according to claim 6, characterized in that: The pH regulator is at least one of hydrochloric acid, sulfuric acid and oxalic acid.

8. The application method of feldspar-quartz flotation separation according to claim 6, characterized in that: The fineness of feldspar and quartz associated ore after crushing and grinding is distributed in the range of 0.075-0.145mm.

9. The application method of feldspar-quartz flotation separation according to claim 6, characterized in that: The mass concentration of the first slurry is 30-45%, the stirring time is 5-10 minutes, and the sedimentation time is 10 minutes.

10. The application method of feldspar-quartz flotation separation according to claim 6, characterized in that: The mass concentration of the second slurry is 50-60%, the pH is adjusted to 9-11, 100-200g of feldspar-quartz flotation combined collector is added per ton of raw ore, stirred, and aerated flotation is performed once to separate feldspar and quartz from the associated ore.

11. The application method of feldspar-quartz flotation separation according to claim 6, characterized in that: Re-adjust the pH to 10-11, add 50-100g of feldspar-quartz flotation combined collector per ton of raw ore, stir, and perform secondary aeration flotation to obtain feldspar and quartz products.

12. The application method of feldspar-quartz flotation separation according to claim 6, characterized in that: The total content of K2O and Na2O in the feldspar product obtained by this method reaches 12.89%, and a large amount of impurity elements such as Al, Ca, Mg, Fe, and Cu are removed, reaching the feldspar grade I standard.

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