A stripping agent for zinc oxide concentrate surface flotation reagent and a preparation method and application thereof

The prepared compound stripping agent removes residual flotation reagents from the surface of zinc oxide concentrate, solving the problems of foaming and excessive TOC during acid leaching of zinc oxide concentrate and improving the treatment effect of zinc oxide concentrate.

CN119076235BActive Publication Date: 2025-11-21KUNMING METALLURGY INST
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Patent Information

Application Number
CN202411072582.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-08-06
Publication Date
2025-11-21
Estimated Expiration
2044-08-06

AI Technical Summary

Technical Problem

Existing technologies are insufficient to effectively remove residual flotation reagents from the surface of zinc oxide concentrate, leading to foaming during acid leaching and excessive TOC content in the leachate, which affects subsequent smelting processes.

Method used

A stripping agent, formulated from a compound of ammonium dodecyl sulfate, butanediol, propylene oxide, and neopentyl glycol dioctanoate, is prepared through steps such as stirring, heating, and ultrasonic emulsification. It is used to adsorb and remove residual flotation reagents from the surface of zinc oxide concentrate.

Benefits of technology

It effectively improves the foaming phenomenon of slurry during acid leaching, reduces the TOC content in the leachate, and improves the stability and economy of subsequent processes.

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Abstract

The application discloses a stripping agent for a zinc oxide concentrate surface flotation reagent and a preparation method and application thereof, and belongs to the technical field of lead-zinc ore dressing. The stripping agent contains, in terms of mass parts, 30-40 parts of ammonium lauryl sulfate, 10-20 parts of butanediol, 20-25 parts of propylene oxide, 30-35 parts of neopentyl glycol dioctanoate and 40-46 parts of water. The water (40-46 parts), the ammonium lauryl sulfate (30-40 parts) and the butanediol (10-20 parts) are added into a reaction kettle, heated and stirred until the reaction material is heated to 35-45 DEG C to obtain a solution a. The propylene oxide (20-25 parts) is added into the solution a, and stirred at room temperature for 1.5-2.5 hours to obtain a solution b. The neopentyl glycol dioctanoate (30-35 parts) is added into the solution b, and stirred at room temperature for 3-5 hours to obtain a solution c. The pH value of the solution c is adjusted to 4-5, and the solution c is ultrasonically emulsified at 40-45 DEG C for 20-40 minutes, and then cooled to room temperature. When used, the stripping agent is added into ore slurry in an amount of 2-5 times, and stirred at 20-30 DEG C for 40-45 minutes. The stripping agent can effectively strip the surface reagent of the oxidized ore, improve the foaming phenomenon during acid leaching, and reduce the TOC content of the leaching solution.
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Description

Technical Field

[0001] This invention belongs to the field of lead-zinc ore beneficiation technology, specifically relating to a stripping agent for surface flotation of zinc oxide concentrate, its preparation method, and its application. Background Technology

[0002] Pingzinc Mine possesses the largest single-unit producing lead-zinc deposit in China and the fifth largest in the world. After years of selective mining and abandonment of lower-grade deposits, the mining area has accumulated 40 million tons of low-grade oxygen-sulfur mixed lead-zinc ore (grades: Zn 6.5%, Pb 1.58%, zinc metal content: 2.1356 million tons, lead metal content: 492,000 tons), accounting for one-third of the current geological reserves. Due to the difficulty in processing and the low grade, this deposit has not been effectively developed.

[0003] Based on years of previous research, obtaining oxygen-sulfur mixed concentrate from low-grade oxygen-sulfur mixed stockpiled ore through mixed flotation has good economic efficiency and process stability. There are two key technical difficulties in the smelting application of this mixed concentrate: (1) Because it is an oxygen-sulfur mixture, it is difficult to enter the existing smelting process flow; (2) After mixed flotation, the oxidized ore is encapsulated and sulfided by flotation reagents (xanthate, No. 2 oil, sodium lignosulfonate, octadecylamine, etc.), and existing mineral processing technology is difficult to separate oxygen and sulfur.

[0004] When the oxide ore obtained after the oxygen-sulfur separation process is directly subjected to acid leaching, bubbles will be generated, and the TOC content in the leachate will exceed the standard. Excessive TOC will lead to rough zinc flakes that are difficult to peel off during the electrolysis stage. To solve these problems, the residual flotation reagents on the surface of the zinc oxide concentrate are pre-treated to remove them, which can improve the foaming phenomenon during acid leaching and reduce the TOC content in the leachate. Summary of the Invention

[0005] The first objective of this invention is to provide a stripping agent for residual flotation reagents on the surface of zinc oxide concentrate; the second objective of this invention is to provide a method for preparing the stripping agent; and the third objective of this invention is to provide the application of the stripping agent in removing residual flotation reagents from the surface of zinc oxide concentrate.

[0006] The first objective of this invention is achieved as follows: the stripping agent comprises, by weight, 30-40 parts of ammonium dodecyl sulfate, 10-20 parts of butanediol, 20-25 parts of propylene oxide, 30-35 parts of neopentyl glycol dioctyl ester, and 40-46 parts of water.

[0007] The second objective of this invention is achieved as follows: the method for preparing the stripping agent includes the following steps:

[0008] Step 1: Add 40-46 parts of water, 30-40 parts of ammonium dodecyl sulfate, and 10-20 parts of butanediol to the reaction vessel in sequence, stirring and heating until the temperature of the reactants in the vessel reaches 35-45℃, to obtain solution a.

[0009] Step 2: Add 20-25 parts of propylene oxide to solution a, stir and react at room temperature for 1.5-2.5 hours to obtain solution b.

[0010] Step 3: Add 30-35 parts of neopentyl glycol dioctanoate to solution b, stir and react at room temperature for 3-5 hours to obtain solution c.

[0011] Step 4: Adjust the pH of solution c to 4-5, then sonicate solution c at 40-45℃ for 20-40 minutes, and cool it to room temperature to obtain the target stripping agent.

[0012] The third objective of this invention is achieved as follows: the stripping agent is used to remove residual flotation reagents from the surface of zinc oxide concentrate by adding the stripping agent to the zinc oxide concentrate slurry at a dosage of 2 to 5 and stirring for 40 to 45 minutes.

[0013] Compared with existing technologies, the technical solution of this invention has outstanding substantive features and significant progress in the following aspects: The stripping agent is formed by compounding ammonium dodecyl sulfate, butanediol, propylene oxide, and neopentyl glycol dioctyl ester. When the stripping agent is added to the zinc oxide concentrate slurry, it exhibits good surface activity, adsorbing residual flotation reagents on the surface of the mineral particles and depositing them onto the groups of the stripping agent. After pressure filtration, the stripping agent carries the beneficiation reagents from the surface of the mineral particles, separating them from the oxide ore with the aqueous solution. The stripping agent can improve the foaming phenomenon of the slurry during acid leaching and simultaneously reduce the TOC content in the leachate. Detailed Implementation

[0014] The present invention will be further described below, but this is not intended to limit the invention in any way. Any modifications or substitutions made based on the teachings of the present invention shall fall within the scope of protection of the present invention.

[0015] The stripping agent of the zinc oxide concentrate surface flotation reagent of the present invention comprises, by weight, 30-40 parts of ammonium dodecyl sulfate, 10-20 parts of butanediol, 20-25 parts of propylene oxide, 30-35 parts of neopentyl glycol dioctanoate, and 40-46 parts of water.

[0016] The stripping agent preferably comprises, by weight, 32 parts ammonium dodecyl sulfate, 16 parts butanediol, 23 parts propylene oxide, 32 parts neopentyl glycol dioctyl ester, and 43 parts water.

[0017] The pH value of the stripping agent is 4 to 5, preferably 4.5.

[0018] The method for preparing the stripping agent includes the following steps:

[0019] Step 1: Add 40-46 parts of water, 30-40 parts of ammonium dodecyl sulfate, and 10-20 parts of butanediol to the reaction vessel in sequence, stirring and heating until the temperature of the reactants in the vessel reaches 35-45℃, to obtain solution a.

[0020] Step 2: Add 20-25 parts of propylene oxide to solution a, stir and react at room temperature for 1.5-2.5 hours to obtain solution b.

[0021] Step 3: Add 30-35 parts of neopentyl glycol dioctanoate to solution b, stir and react at room temperature for 3-5 hours to obtain solution c.

[0022] Step 4: Adjust the pH of solution c to 4-5, then sonicate solution c at 40-45℃ for 20-40 minutes, and cool it to room temperature to obtain the target stripping agent.

[0023] The heating rate mentioned in step 1 is 3~6℃ / min.

[0024] The preferred reaction time in step 2 is 2 hours.

[0025] The preferred reaction time in step 3 is 4 hours.

[0026] The preferred ultrasonic emulsification time in step 4 is 30 minutes.

[0027] The stripping agent is used to remove the flotation reagent from the surface of zinc oxide concentrate during the separation stage. The stripping agent is added to the zinc oxide concentrate slurry at a dosage of 2 to 5, and stirred at 20 to 30°C for 40 to 45 minutes.

[0028] Example 1

[0029] The stripping agent of the zinc oxide concentrate surface flotation reagent comprises 35g of ammonium dodecyl sulfate, 15g of butanediol, 22g of propylene oxide, 35g of neopentyl glycol dioctanoate, and 43g of water, with a pH value of 4.5.

[0030] The stripping agent is prepared by:

[0031] Step 1: Add 43g of water, 35g of ammonium dodecyl sulfate, and 15g of butanediol to the reaction vessel in sequence, and heat while stirring. The temperature is increased at a rate of 5℃ / min until the reactants in the vessel reach 40℃, resulting in a homogeneous solution a.

[0032] Step 2: Slowly add 22g of propylene oxide dropwise to solution a, and stir the reaction at room temperature for 2 hours to obtain solution b.

[0033] Step 3: Slowly add 35g of neopentyl glycol dioctanoate to solution b, and stir the reaction at room temperature for 4 hours to obtain solution c.

[0034] Step 4: Adjust the pH of solution c to 4.5, then sonicate solution c at 42℃ for 30 minutes, and cool it to room temperature to obtain the target stripping agent.

[0035] The application method of the stripping agent is as follows:

[0036] The prepared stripping agent was added to the zinc oxide concentrate slurry at a dosage of 4, and stirred at 25°C for 40 minutes.

[0037] Example 2

[0038] The stripping agent of the zinc oxide concentrate surface flotation reagent comprises 30g of ammonium dodecyl sulfate, 12g of butanediol, 25g of propylene oxide, 33g of neopentyl glycol dioctanoate, and 40g of water, with a pH value of 4.

[0039] The stripping agent is prepared by:

[0040] Step 1: Add 40g of water, 30g of ammonium dodecyl sulfate, and 12g of butanediol to the reaction vessel in sequence, and heat while stirring at a rate of 4℃ / min until the reactants in the vessel reach 45℃, to obtain a homogeneous solution a.

[0041] Step 2: Slowly add 25g of propylene oxide dropwise to solution a, and stir the reaction at room temperature for 2.5h to obtain solution b.

[0042] Step 3: Slowly add 33g of neopentyl glycol dioctanoate to solution b, and stir the reaction at room temperature for 5 hours to obtain solution c.

[0043] Step 4: Adjust the pH of solution c to 4, then sonicate solution c at 45℃ for 20 minutes, and cool it to room temperature to obtain the target stripping agent.

[0044] The application method of the stripping agent is as follows:

[0045] During the sorting stage, the prepared stripping agent was added to the zinc oxide concentrate slurry at a dosage of 3 and stirred at 28°C for 45 minutes.

[0046] Example 3

[0047] The stripping agent of the zinc oxide concentrate surface flotation reagent comprises 40g of ammonium dodecyl sulfate, 20g of butanediol, 20g of propylene oxide, 30g of neopentyl glycol dioctanoate, and 40g of water, with a pH value of 5.

[0048] The stripping agent is prepared by:

[0049] Step 1: Add 40g of water, 40g of ammonium dodecyl sulfate, and 20 parts of butanediol to the reaction vessel in sequence, and heat while stirring. The temperature is increased at a rate of 4℃ / min until the reactants in the vessel reach 35℃, resulting in a homogeneous solution a.

[0050] Step 2: Slowly add 20g of propylene oxide dropwise to solution a, and stir the reaction at room temperature for 1.5h to obtain solution b.

[0051] Step 3: Slowly add 30g of neopentyl glycol dioctanoate to solution b, and stir the reaction at room temperature for 3 hours to obtain solution c.

[0052] Step 4: Adjust the pH of solution c to 5, then sonicate solution c at 40℃ for 40 min, and cool it to room temperature to obtain the target stripping agent.

[0053] The application method of the stripping agent is as follows:

[0054] During the sorting stage, the prepared stripping agent was added to the zinc oxide concentrate slurry at a dosage of 2 and stirred at 30°C for 42 minutes.

[0055] Example 4

[0056] —Comparison Example

[0057] The stripping agent used as a control example contained 25g of ammonium dodecyl sulfate, 25g of butanediol, 30g of propylene oxide, 25g of neopentyl glycol dioctanoate, and 55g of water, with a pH of 4.5.

[0058] The stripping agent is prepared by:

[0059] Step 1: Add 55g of water, 25g of ammonium dodecyl sulfate, and 25g of butanediol to the reaction vessel in sequence, and heat while stirring. The heating rate is the same as in Example 1, until the reactants in the vessel reach 40°C to obtain a homogeneous solution a.

[0060] Step 2: Slowly add 30g of propylene oxide dropwise to solution a, and stir the mixture at room temperature for 2 hours to obtain solution b.

[0061] Step 3: Slowly add 25g of neopentyl glycol dioctanoate to solution b, and stir the reaction at room temperature for 4 hours to obtain solution c.

[0062] Step 4: Adjust the pH of solution c to 4.5, then sonicate solution c at 42℃ for 30 min, and cool it to room temperature to obtain the stripping agent as a control example.

[0063] The application method of the stripping agent is the same as in Example 1.

[0064] Example 5

[0065] —Comparison of the application effects of the stripping agents prepared in Examples 1, 2, 3 and the control example

[0066] The application method of the stripping agent was uniformly adopted according to the values ​​in Example 1. The TOC content in the leachate was determined according to HJ501—2009 (Determination of Total Organic Carbon in Water - Combustion Oxidation-Non-Dispersive Infrared Absorption Method) standard. The results are shown in the table below:

[0067] .

Claims

1. A stripping agent for surface flotation of zinc oxide concentrate, characterized in that, The stripping agent, by weight, comprises 30-40 parts of ammonium dodecyl sulfate, 10-20 parts of butanediol, 20-25 parts of propylene oxide, 30-35 parts of neopentyl glycol dioctanoate, and 40-46 parts of water.

2. The stripping agent according to claim 1, characterized in that, The pH value of the stripping agent is 4-5.

3. A method for preparing the stripping agent according to claim 1, characterized in that... Includes the following steps: Step 1: Add 40-46 parts of water, 30-40 parts of ammonium dodecyl sulfate, and 10-20 parts of butanediol to the reaction vessel in sequence, stirring and heating until the temperature of the reactants in the vessel rises to 35-45℃, to obtain solution a; Step 2: Add 20-25 parts of propylene oxide to solution a, stir and react at room temperature for 1.5-2.5 hours to obtain solution b; Step 3: Add 30-35 parts of neopentyl glycol dioctanoate to solution b, stir and react at room temperature for 3-5 hours to obtain solution c; Step 4: Adjust the pH of solution c to 4-5, then sonicate solution c at 40-45℃ for 20-40 minutes, and cool it to room temperature to obtain the target stripping agent.

4. The preparation method according to claim 3, characterized in that, The heating rate mentioned in step 1 is 3~6℃ / min.

5. The preparation method according to claim 3, characterized in that, The reaction time described in step 2 is 2 hours.

6. The preparation method according to claim 3, characterized in that, The reaction time described in step 3 is 4 hours.

7. The preparation method according to claim 3, characterized in that, The ultrasonic emulsification time in step 4 is 30 minutes.

8. The application of the stripping agent according to claim 1 in removing surface flotation reagents from zinc oxide concentrate, characterized in that, During the sorting stage, the stripping agent is added to the zinc oxide concentrate slurry at a dosage of 2-5, and stirred at 20-30℃ for 40-45 minutes.

Citation Information

Patent Citations

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  • Selection method of high mud lead zinc oxide sulfur mixed ores

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