Chalcopyrite floating composite collector and application thereof

By preparing a composite collector generated by the reaction of cyclic ketones and hydroxylamine compounds with potassium amylxanthate, benzoyl chloride, etc., the problems of pipeline calcium deposition and environmental pollution caused by the high alkaline environment in chalcopyrite flotation were solved, and efficient recovery of chalcopyrite and reduction of the pH value of tailings were achieved, thereby improving the grade of copper concentrate and corporate benefits.

CN116689156BActive Publication Date: 2025-10-21安徽铜冠产业技术研究院有限责任公司
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Patent Information

Application Number
CN202310717721.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-15
Publication Date
2025-10-21
Estimated Expiration
2043-06-15

AI Technical Summary

Technical Problem

In the existing chalcopyrite flotation technology, the high alkaline environment leads to a high risk of calcium deposition in pipelines, low economic benefits, and poor environmental sustainability. In addition, the pH value of the tailings wastewater is too high, making it difficult to effectively recover chalcopyrite in a low-alkaline environment.

Method used

A composite collector consisting of a first collector prepared from a cyclic ketone compound and a hydroxylamine compound and a second collector prepared from potassium amyl xanthate and benzoyl chloride is used to generate a chalcopyrite flotation reagent with high selectivity and strong collecting ability through chemical reaction for chalcopyrite flotation.

Benefits of technology

Significantly improve the recovery rate and copper grade of chalcopyrite in a low-alkaline environment, reduce the incorporation of sulfur minerals, lower the pH value of tailings return water, meet environmental emission standards, and enhance the company's economic benefits and environmental sustainability.

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Abstract

The present application relates to the technical field of mineral flotation reagent, in particular to a chalcopyrite flotation composite collector and application thereof; the chalcopyrite flotation composite collector is prepared by mixing a first collector and a second collector at a mass ratio of 5-7:1.0-1.5; the prepared first collector is applied to the field of chalcopyrite flotation, and has good flotation performance and higher selectivity, and significantly improves the recovery rate of chalcopyrite flotation; the obtained second collector contains multiple sulfur-containing and oxygen-containing functional groups in the molecule, has good collecting ability and selectivity for chalcopyrite, and can significantly improve the flotation recovery rate of chalcopyrite; in addition, the mutual cooperation between the first collector and the second collector can further improve the recovery rate and grade of chalcopyrite; under the condition of adding a small amount of lime, a copper concentrate with high copper grade is obtained, the pH value of tailing backwater is also greatly reduced, the alkalinity standard requirement of direct discharge of backwater is met, and the sustainable development of the environment is beneficial.
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Description

Technical Field

[0001] The invention relates to the technical field of copper mineral flotation reagents, in particular to a chalcopyrite flotation composite collector and application thereof. Background Art

[0002] Chalcopyrite is a common copper-iron sulfide mineral. Its crystals are relatively rare and tetrahedral. They are mostly irregular granular and dense massive aggregates, as well as kidney-shaped and grape-shaped aggregates. It is copper-yellow, often with dark yellow or spotted ochre color. The streak is slightly greenish black. Chalcopyrite can be formed in different environments, but it is mainly the product of hydrothermal action and contact metasomatism. It can often form deposits of a certain scale, and its production areas are all over the world. In industry, it is the main raw material for copper smelting. It often contains trace amounts of rare and precious metals such as gold and silver.

[0003] Chalcopyrite's most common associated mineral is pyrite. In production applications, large amounts of lime are typically added to create a highly alkaline environment to inhibit the hydrophobic flotation of pyrite, and collectors with strong capture properties are used to flotate the chalcopyrite. This method is simple to apply and widely applicable, but due to the large amount of lime added, long-term use can increase the risk of calcium buildup in pipelines. Furthermore, the highly alkaline flotation environment can inhibit the recovery of associated gold minerals, significantly reducing the company's economic benefits. Furthermore, the high pH value of the tailings wastewater can also have certain impacts on environmental sustainability.

[0004] Currently, in practical production applications, to avoid adding large amounts of lime in the roughing process, copper mineral flotation is often performed in a weakly alkaline environment during the roughing process. During the concentrating and middling separation processes, a high-alkaline environment is created to suppress pyrite. Although the tailings return water concentration is significantly reduced, it is still above the normal pH discharge limit of 9.0. Based on this, the present invention provides a composite collector for chalcopyrite flotation and its application to address this technical problem. Summary of the Invention

[0005] The present invention provides a composite collector for chalcopyrite flotation and its application. The first collector of the present invention exhibits excellent flotation performance when applied to chalcopyrite flotation, significantly improving the flotation recovery rate of chalcopyrite. The prepared second collector, containing multiple sulfur- and oxygen-containing functional groups in its molecule, exhibits excellent chalcopyrite capture and selectivity, significantly improving the copper grade of chalcopyrite. Furthermore, the first and second collectors work synergistically, and further produce a synergistic effect with butyl xanthate, thereby improving the recovery rate and grade of chalcopyrite.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A chalcopyrite flotation composite collector is prepared by mixing a first collector and a second collector in a mass ratio of 5-7:1.0-1.5.

[0008] The preparation method of the first collector comprises the following steps:

[0009] Step 1: Add equimolar amounts of a cyclic ketone compound and a hydroxylamine compound into a reaction kettle, then add an organic solvent 3 to 6 times the mass of the cyclic ketone compound into the reaction kettle, mix and stir evenly, raise the temperature of the obtained first mixed component to 85 to 105° C., and keep the reaction at this temperature for 3 to 5 hours;

[0010] Step 2: After the reaction is completed, add 1.2 to 1.6 times the mass of methanol to the resulting product component, mix and stir evenly, and then slowly dropwise add 1.0 to 1.8 times the molar amount of carbon disulfide to the resulting second mixed solution, mix and stir evenly, and then heat the resulting third mixed solution at 3 to 8° C. and stir for 3 to 6 hours;

[0011] Step 3: After the reaction is completed, add sodium hydroxide with a mass of 0.5 to 0.7 times that of carbon disulfide to the resulting component, and add bromooctane with a mass of 3 to 4 times that of sodium hydroxide at a temperature of 10 to 20° C. while stirring, and keep the reaction warm for 12 to 18 hours;

[0012] Step 4: After the reaction is completed, the temperature of the reaction product is naturally cooled to below 3°C, and the pH thereof is adjusted to 3.5-4.2; finally, the product is filtered, distilled under reduced pressure, washed with deionized water, and dried under vacuum to obtain the first collector product.

[0013] Furthermore, the cyclic ketone compound is cyclohexanone isoxime.

[0014] Furthermore, the hydroxylamine compound is selected from any one of hydroxylamine chloride and hydroxylamine sulfate.

[0015] Furthermore, the organic solvent is toluene.

[0016] Furthermore, in the step 2, the temperature of the mixed phase is always lower than 8°C when carbon disulfide is added dropwise.

[0017] Furthermore, the preparation method of the second collector includes the following steps: transferring equimolar amounts of potassium amyl xanthate and benzoyl chloride into a reactor, adding methylene chloride with a volume 2.5 to 4 times that of benzoyl chloride to the reactor, mixing and stirring evenly, raising the temperature of the resulting mixed liquid to 15 to 25°C, and stirring and reacting at this temperature for 2 to 3 hours; after the reaction is completed, filtering out the sodium chloride in the resulting product components, and recovering the solvent in the remaining filtrate by vacuum distillation, and the final product is the second collector product.

[0018] Furthermore, the mixing rate in step 1 is set to 300-500 r / min, and the mixing time is set to 30-40 min.

[0019] Furthermore, during the vacuum drying in step 4, the temperature in the drying oven is set to 60-75°C.

[0020] Furthermore, the chalcopyrite flotation composite collector is applied to the chalcopyrite flotation field, and the amount of the composite collector used relative to the chalcopyrite during the flotation process is 20-60 g / t, and the pH value of the pulp is 7.5-9.0.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] 1. The present invention uses cyclic ketone compounds and hydroxylamine compounds as raw materials, and after heat preservation reaction, prepares a hydroxamic acid compound with an amino group connected to the molecular chain, which has high selectivity for metal ions. Then, the hydroxamic acid compound is combined with carbon disulfide, octyl bromide, etc. as raw materials, and a first collector with strong adsorption strength and capture capacity is prepared through a chemical reaction between the raw materials. The prepared first collector is applied to the field of chalcopyrite flotation and not only has good flotation performance and higher selectivity, but also has a strong chelating ability for copper ions, significantly improving the recovery rate of chalcopyrite flotation.

[0023] 2. The present invention also uses potassium amyl xanthate, benzoyl chloride, and methylene chloride as raw materials. A chemical reaction between potassium amyl xanthate and benzoyl chloride produces a xanthate acyl ester, which is then filtered to remove sodium chloride and subjected to vacuum distillation to produce a second collector with high purity. The resulting second collector contains multiple sulfur- and oxygen-containing functional groups in its molecule, exhibits excellent capture and selectivity for chalcopyrite, and can significantly improve the flotation recovery rate of chalcopyrite. Furthermore, the synergistic effect between the first and second collectors can further improve the recovery rate of chalcopyrite and the copper grade.

[0024] 3. The chalcopyrite composite flotation collector proposed in the present invention can replace some existing collectors in low-alkaline environments, selectively improve the copper grade of flotation foam, reduce the incorporation of sulfur minerals, and achieve the goal of obtaining a copper concentrate with a higher copper grade by adding a small amount of lime. It can also significantly reduce the pH value of tailings return water to meet the alkalinity standard requirements for direct discharge of return water, which is conducive to environmental sustainability. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a test flow chart of Examples 1 to 3 and Comparative Examples 1 to 2 of the present invention, i.e., a one-coarse and two-fine process under room temperature conditions;

[0026] Figure 2 This is a process flow chart of Application Example 1 of the present invention. DETAILED DESCRIPTION

[0027] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only 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 making any creative efforts shall fall within the scope of protection of the present invention.

[0028] Example 1

[0029] A chalcopyrite flotation composite collector is prepared by mixing a first collector and a second collector in a mass ratio of 6:1.2.

[0030] The preparation method of the first collector comprises the following steps:

[0031] Step 1: adding equimolar amounts of cyclohexanone isoxime and hydroxylamine sulfate into a reactor, then adding toluene in an amount 5 times the mass of cyclohexanone isoxime into the reactor, mixing and stirring uniformly, raising the temperature of the obtained first mixed component to 95° C., and keeping the mixture at this temperature for 4 hours; wherein the mixing and stirring rate is set to 400 r / min, and the mixing and stirring time is set to 35 minutes;

[0032] Step 2: After the reaction is completed, methanol with a mass 1.4 times that of the product component is added to the obtained product component, and after mixing and stirring evenly, carbon disulfide with a molar amount 1.5 times that of hydroxyl sulfate is slowly added dropwise to the obtained second mixed solution, and after mixing and stirring evenly, the obtained third mixed solution is kept stirred at a temperature of 5°C for 4h; wherein, the temperature of the mixed phase is always below 8°C when carbon disulfide is added dropwise.

[0033] Step 3: After the reaction is completed, add sodium hydroxide with a mass of 0.6 times that of carbon disulfide to the resulting component, and add bromooctane with a mass of 3.5 times that of sodium hydroxide at a temperature of 15°C while stirring, and keep the reaction warm for 15 hours;

[0034] Step 4: After the reaction is completed, the temperature of the reaction product is naturally cooled to below 3°C, and the pH thereof is adjusted to 4.0; finally, the product is filtered, distilled under reduced pressure, washed with deionized water, and vacuum dried to obtain the first collector product; wherein, the temperature in the drying oven is set to 70°C during vacuum drying.

[0035] The preparation method of the second collector comprises the following steps: transferring equimolar amounts of potassium amyl xanthate and benzoyl chloride into a reactor, adding methylene chloride in a volume three times that of benzoyl chloride into the reactor, mixing and stirring uniformly, raising the temperature of the resulting mixed liquid to 20° C., and stirring and reacting at this temperature for 2.5 hours; after the reaction is completed, filtering out sodium chloride from the resulting product components, and recovering the solvent in the remaining filtrate through reduced pressure distillation, thereby obtaining the final product of the second collector.

[0036] During the flotation process, the dosage of the composite collector relative to the original ore is 40g / t, and the pH value of the pulp is 7.5.

[0037] Example 2

[0038] A chalcopyrite flotation composite collector is prepared by mixing a first collector and a second collector in a mass ratio of 5:1.

[0039] The preparation method of the first collector comprises the following steps:

[0040] Step 1: adding equimolar amounts of cyclohexanone isoxime and hydroxylamine chloride into a reactor, then adding toluene in an amount 3 times the mass of cyclohexanone isoxime into the reactor, mixing and stirring uniformly, raising the temperature of the obtained first mixed component to 85° C., and keeping the mixture at this temperature for 3 hours; wherein the mixing and stirring rate is set to 300 r / min, and the mixing and stirring time is set to 30 minutes;

[0041] Step 2: After the reaction is completed, add 1.2 times the mass of methanol to the obtained product component, mix and stir evenly, and then slowly dropwise add carbon disulfide in an amount equimolar to hydroxylamine chloride to the obtained second mixed solution, mix and stir evenly, and then heat the obtained third mixed solution at 3°C ​​and stir for 3 hours; wherein, the temperature of the mixed phase is always below 8°C when adding carbon disulfide;

[0042] Step 3: After the reaction is completed, add sodium hydroxide with a mass of 0.5 times that of carbon disulfide to the resulting component, and add bromooctane with a mass of 3 times that of sodium hydroxide at a temperature of 10°C while stirring, and keep the reaction warm for 12 hours;

[0043] Step 4: After the reaction is completed, the temperature of the reaction product is naturally cooled to below 3°C, and the pH thereof is adjusted to 3.5; finally, the product is filtered, distilled under reduced pressure, washed with deionized water, and vacuum dried to obtain the first collector product; wherein, the temperature in the drying oven is set to 60°C during vacuum drying.

[0044] The preparation method of the second collector comprises the following steps: transferring equimolar amounts of potassium amyl xanthate and benzoyl chloride into a reactor, adding methylene chloride in a volume 2.5 times that of benzoyl chloride into the reactor, mixing and stirring uniformly, raising the temperature of the resulting mixed liquid to 15° C., and stirring and reacting at this temperature for 2 hours; after the reaction is completed, filtering out sodium chloride from the resulting product components, and recovering the solvent in the remaining filtrate through reduced pressure distillation, thereby obtaining the final product of the second collector.

[0045] During the flotation process, the dosage of the composite collector relative to the original ore is 20 g / t, and the pH value of the pulp is 8.0.

[0046] Example 3

[0047] A chalcopyrite flotation composite collector is prepared by mixing a first collector and a second collector in a mass ratio of 7:1.5.

[0048] The preparation method of the first collector comprises the following steps:

[0049] Step 1: adding equimolar amounts of cyclohexanone isoxime and hydroxylamine chloride into a reactor, then adding toluene in an amount 6 times the mass of cyclohexanone isoxime into the reactor, mixing and stirring uniformly, raising the temperature of the obtained first mixed component to 105° C., and keeping the mixture at this temperature for 5 hours; wherein the mixing and stirring rate is set to 500 r / min, and the mixing and stirring time is set to 40 minutes;

[0050] Step 2: After the reaction is completed, methanol in an amount 1.6 times the mass of the product component is added to the obtained product component, and after mixing and stirring, carbon disulfide in an amount 1.8 times the molar amount of hydroxylamine chloride is slowly added dropwise to the obtained second mixed solution, and after mixing and stirring, the obtained third mixed solution is kept at 8° C. and stirred for 6 hours; wherein, the temperature of the mixed phase is always below 8° C. when carbon disulfide is added dropwise;

[0051] Step 3: After the reaction is completed, add sodium hydroxide with a mass of 0.7 times that of carbon disulfide to the resulting component, and add bromooctane with a mass of 4 times that of sodium hydroxide at a temperature of 20°C while stirring, and keep the reaction warm for 18 hours;

[0052] Step 4: After the reaction is completed, the temperature of the reaction product is naturally cooled to below 3°C, and the pH thereof is adjusted to 4.2; finally, the product is filtered, distilled under reduced pressure, washed with deionized water, and vacuum dried to obtain the first collector product; wherein, the temperature in the drying oven is set to 75°C during vacuum drying.

[0053] The preparation method of the second collector comprises the following steps: transferring equimolar amounts of potassium amyl xanthate and benzoyl chloride into a reactor, adding methylene chloride in a volume four times that of benzoyl chloride into the reactor, mixing and stirring uniformly, raising the temperature of the resulting mixed liquid to 25° C., and stirring and reacting at this temperature for 3 hours; after the reaction is completed, filtering out sodium chloride from the resulting product components, and recovering the solvent in the remaining filtrate through reduced pressure distillation, thereby obtaining the final product of the second collector.

[0054] During the flotation process, the dosage of the composite collector relative to the original ore is 60g / t, and the pH value of the pulp is 9.0.

[0055] Comparative Example 1: The difference from Example 1 is that in this example, an equal amount of the first collector is used instead of the second collector;

[0056] Comparative Example 2: The difference from Example 1 is that in this example, an equal amount of the second collector is used instead of the first collector;

[0057] In combination with Examples 1 to 3 and Comparative Examples 1 to 2, the provided chalcopyrite flotation composite collector was used to conduct a flotation test on an ore in Anhui Province in which chalcopyrite and pyrite were in a symbiotic relationship (one coarse and two fine operations under room temperature), and the obtained data were recorded in Table 1:

[0058] Table 1: Comparative results of chalcopyrite flotation reagent performance test;

[0059]

[0060]

[0061] By comparing and analyzing the relevant data in Table 1, it can be seen that the first collector prepared by the present invention, when applied to the chalcopyrite flotation field, not only has good flotation performance, but also has higher selectivity, significantly improving the flotation recovery rate of chalcopyrite; the second collector prepared contains multiple sulfur-containing and oxygen-containing functional groups in its molecule, has good capture ability and selectivity for chalcopyrite, and can significantly improve the flotation recovery rate of chalcopyrite. Furthermore, the mutual synergy between the first collector and the second collector can further improve the recovery rate and grade of chalcopyrite. Therefore, it is shown that the chalcopyrite flotation composite collector provided by the present invention has a broader market prospect and is more suitable for promotion.

[0062] Application Example 1: The chalcopyrite flotation composite collector in Example 1 is applied to a copper sulfide mine in Anhui Province, and the attached figure of the specification is used. Figure 2 The provided process is used to process copper ore. The copper grade of the raw ore is about 0.425%. The copper sulfide minerals in the raw ore are mainly chalcopyrite, which is symbiotic with pyrite. The commonly used production process in this field at this stage is semi-priority flotation + mixed middling separation process, and butyl xanthate is generally used as the collector. The amount of lime added in the semi-priority roughing operation is 0.8kg / t. The chalcopyrite flotation composite collector is added at a dosage of 20g / t. The scavenging operation adopts a mixture of butyl xanthate and composite collector, and the addition mass ratio is 3:1. No lime is added in the semi-priority selection operation. The amount of lime added in the separation operation after middling regrinding is 0.6kg / t. The amount of lime added in the two-stage separation and selection is 100g / t. The test results are shown in Table 2:

[0063] Table 2: Flotation test indicators of Example 1;

[0064]

[0065]

[0066] The test results show that in Example 1, 0.8 g / t of lime was added in the semi-priority roughing operation, and no lime was added in the semi-priority concentration operation, and a copper concentrate 1 with a copper grade of 29.78% was obtained. The slurry pH value of the tailings 1 was about 8.6. The amount of lime added in the separation roughing operation after regrinding the middlings was 1 kg / t, and the amount of lime added in the two-stage separation and concentration operations was 100 g / t. A copper concentrate 2 with a copper grade of 11.78% was obtained, the copper grade of the ∑ copper concentrate was 21.12%, the slurry pH value of the tailings 2 was about 11.5, and the slurry pH value of the ∑ tailings could be stabilized below 9.0.

[0067] Application Example 2: The difference from Application Example 1 is that in Application Example 2, an equal amount of butyl xanthate is used instead of the chalcopyrite flotation composite collector, and the amount of lime added remains unchanged. The test results are shown in Table 3:

[0068] Table 3: Flotation test indicators of comparative example 3;

[0069] Product Name Yield / % Copper grade / % Copper recovery rate / % Copper concentrate 1 1.03 28.25 68.67 Copper concentrate 2 1.24 8.38 24.52 ∑Copper concentrate 2.27 17.40 93.19 Tailings 1 93.68 0.026 5.75 Tailings 2 4.05 0.111 1.06 ∑ tailings 98.13 0.030 6.81 raw ore 100.00 0.424 100.00

[0070] The test results show that after an equal amount of butyl xanthate was used instead of the chalcopyrite flotation composite collector in the semi-priority roughing operation, the grade of copper concentrate 1 dropped to 28.25%. Moreover, due to the poor selectivity of the collector, a large amount of pyrite was mixed into the middlings. When the lime addition amount after regrinding was still 1 kg / t, the copper concentrate 2 was doped with a certain amount of pyrite, resulting in a significant drop in the copper grade of copper concentrate 2 to 8.38%, and the copper grade of the ∑ copper concentrate dropped to 17.40%.

[0071] Application Example 3: The difference from Application Example 1 is that in Application Example 3, an equal amount of butyl xanthate is used instead of the chalcopyrite flotation composite collector. Lime is added in a dosage of 300g / t during the semi-preferential concentrating operation, and the amount of lime added after regrinding the middlings is increased to 1.5kg / t. This reagent system is the actual production reagent system on site. The test results are shown in Table 4:

[0072] Table 4: Flotation test indicators of Comparative Example 4;

[0073] Product Name Yield / % Copper grade / % Copper recovery rate / % Copper concentrate 1 0.97 29.89 68.23 Copper concentrate 2 0.92 11.62 25.16 ∑Copper concentrate 1.89 20.95 93.39 Tailings 1 93.85 0.025 5.52 Tailings 2 4.26 0.109 1.09 ∑ tailings 98.13 0.030 6.61 raw ore 100.00 0.425 100.00

[0074] The test results show that in Application Example 3, an equal amount of butyl xanthate is used instead of the chalcopyrite flotation composite collector in the semi-priority roughing operation. After adding 300g / t of lime in the semi-priority concentrating operation, a copper concentrate 1 with a copper grade of 29.89% can be obtained, and the slurry pH value of the tailings 1 does not change. At the same time, after the lime addition amount is increased to 1.5kg / t after the middlings are regrinded, a copper concentrate 2 with a copper grade of 11.62% can be obtained, and the ∑ copper concentrate grade is 20.95%, which is similar to the test results of Example 1. However, the slurry pH value of the tailings 2 increases to 12.2, and the slurry pH value of the ∑ tailings increases to about 10.3. Although a copper concentrate with good separation indicators is obtained, the high pH value of the tailings backwater will have a certain impact on environmental sustainability. In addition, the increased amount of lime addition will also inhibit the floatability of gold minerals and increase the risk of calcium deposition in pipelines.

[0075] Based on the test results of Application Examples 1 to 3, the chalcopyrite flotation composite collector proposed in the present invention can replace part of conventional collectors in a low-alkali environment. It can also use its better selectivity to improve the copper grade of flotation foam, reduce the incorporation of sulfur minerals, and achieve a copper concentrate with a higher copper grade by adding a small amount of lime. It can also significantly reduce the pH value of tailings backwater, meet the alkalinity standard requirements for direct discharge of backwater, and is conducive to environmental sustainability.

[0076] Throughout this specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

[0077] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to the specific embodiments described. Obviously, many modifications and variations are possible based on the content of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A method for preparing a composite collector for chalcopyrite flotation, characterized in that the composite collector for chalcopyrite flotation is composed of a first collector and a second collector in a ratio of 5 to 7: Mixed and compounded in a mass ratio of 1.0 to 1.5; The preparation method of the first collector comprises the following steps: Step 1: Add equimolar amounts of a cyclic ketone compound and a hydroxylamine compound into a reaction kettle, then add an organic solvent 3 to 6 times the mass of the cyclic ketone compound into the reaction kettle, mix and stir evenly, raise the temperature of the obtained first mixed component to 85 to 105° C., and keep the reaction at this temperature for 3 to 5 hours; Step 2: After the reaction is completed, add 1.2 to 1.6 times the mass of methanol to the resulting product component, mix and stir evenly, and then slowly dropwise add 1.0 to 1.8 times the molar amount of carbon disulfide to the resulting second mixed solution, mix and stir evenly, and then heat the resulting third mixed solution at 3 to 8° C. and stir for 3 to 6 hours; Step 3: After the reaction is completed, add sodium hydroxide with a mass of 0.5 to 0.7 times that of carbon disulfide to the resulting component, and add bromooctane with a mass of 3 to 4 times that of sodium hydroxide at a temperature of 10 to 20° C. while stirring, and keep the reaction warm for 12 to 18 hours; Step 4: After the reaction is completed, the temperature of the reaction product is naturally cooled to below 3°C, and the pH thereof is adjusted to 3.5-4.2; finally, the product is filtered, distilled under reduced pressure, washed with deionized water, and vacuum dried to obtain the first collector product; The preparation method of the second collector comprises the following steps: transferring equimolar amounts of potassium amyl xanthate and benzoyl chloride into a reactor, adding methylene chloride in a volume 2.5 to 4 times that of benzoyl chloride into the reactor, mixing and stirring uniformly, raising the temperature of the resulting mixed liquid to 15 to 25° C., and stirring and reacting at this temperature for 2 to 3 hours; after the reaction is completed, filtering out sodium chloride from the resulting product components, and recovering the solvent in the remaining filtrate by vacuum distillation, thereby obtaining the final product of the second collector.

2. The method for preparing a chalcopyrite flotation composite collector according to claim 1, wherein: The cyclic ketone compound is cyclohexanone isoxime.

3. The method for preparing a chalcopyrite flotation composite collector according to claim 1, wherein: The hydroxylamine compound is selected from any one of hydroxylamine chloride and hydroxyl sulfate.

4. The method for preparing a chalcopyrite flotation composite collector according to claim 1, wherein: The organic solvent is toluene.

5. The method for preparing a chalcopyrite flotation composite collector according to claim 1, wherein: In the step 2, the temperature of the mixed phase is always lower than 8° C. when carbon disulfide is added dropwise.

6. The method for preparing a composite collector for chalcopyrite flotation according to claim 1, wherein: The mixing rate in step 1 is set to 300-500 r / min, and the mixing time is set to 30-40 min.

7. The method for preparing a composite collector for chalcopyrite flotation according to claim 1, wherein: During the vacuum drying in step 4, the temperature in the drying oven is set to 60-75°C.

8. Use of the composite collector for chalcopyrite flotation prepared by the method according to any one of claims 1 to 7, characterized in that: The chalcopyrite flotation composite collector is applied to the chalcopyrite flotation field, and during the flotation process, the amount of the composite collector used relative to the chalcopyrite is 20-60 g / t, and the pH value of the pulp is 7.5-9.0.

Citation Information

Patent Citations

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