An oil-water separation promoter for alkaline etching waste liquid extraction process

Abstract

The present application relates to a kind of oil-water separation promoters for alkaline etching waste liquid extraction process, with the total mass percentage content being 100wt%, the oil-water separation promoter includes: ethylene glycol monobutyl ether 60-90wt%, the rest is nonylphenol polyoxyethylene ether.The present application will destroy the double electric layer on the surface of emulsified microparticle by designing the oil-water separation promoter of specific component and content, so as to speed up oil-water separation and make separation more thorough, significantly improve production efficiency, reduce the loss of extraction oil, avoid the problem of extraction oil and etching subliquid residual impurities, avoid the adverse effects caused by impurities on etching subliquid reuse, also without changing the existing process equipment, simple and convenient operation.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of extraction, in particular to an oil-water separation promoter for alkaline etching waste liquid extraction process. BACKGROUND

[0002] The extraction process is to mix the aqueous solution and the mixture of the extractant and the solvent oil, and then to separate the layers after standing. The extracted components are transferred from the aqueous solution to the oil phase. The back extraction process is to mix the mixture of the extractant and the solvent oil and the back extraction liquid, and then to separate the layers after standing. The extracted components are transferred from the oil phase to the back extraction liquid. In the operation process of extraction and back extraction, the mixture of the extractant and the solvent oil and the aqueous solution are not miscible and have different specific gravities. The oil and water are separated after standing.

[0003] At present, the existing technology mainly improves the extraction method or the extraction device involved in the extraction process to improve the mixing degree and the extraction efficiency of the raw materials. CN 211836421U discloses a novel extraction separation device, which comprises a support, a jacketed extraction kettle, a horizontal condenser, a vertical condenser, an oil-water separator, an essential oil tank and a pure distillate tank. The upper end of the steam pipe is fixedly connected with the inlet of the horizontal condenser. The lower end of the horizontal condenser is fixedly connected with a reflux pipe. The lower end of the reflux pipe is connected with the lower end of the steam pipe. The upper end of the horizontal condenser is connected with the inlet of the vertical condenser. The outlet of the vertical condenser is connected with the upper end of the oil-water separator. The first oil separation pipe is arranged on the side of the oil-water separator. The lower end of the first oil separation pipe is fixedly connected with the upper end of the essential oil tank. The pure distillate separation pipe is arranged on the lower end of the oil-water separator. The lower end of the pure distillate separation pipe is fixedly connected with the upper end of the pure distillate tank.

[0004] CN 114538554A discloses an extraction method and equipment for hydrometallurgy and oil-water separation of oily sewage. The extraction equipment for hydrometallurgy comprises an extraction container, an extractant inlet pipe, a water phase inlet pipe, a pipeline mixer arranged after the extractant inlet pipe and the water phase inlet pipe for preliminary mixing of the two phases, a water separator arranged in the extraction container and connected with the pipeline mixer, a filter element arranged in the extraction container and connected with the water separator, an extraction liquid outlet pipe connected with the upper end of the extraction container, and a raffinate liquid outlet pipe connected with the lower end of the extraction container.

[0005] However, the extraction device or the extraction method disclosed in the above content does not involve the solution to the oil-water emulsification. In addition, for specific application environments such as the alkaline etching waste liquid extraction and regeneration process, the above-mentioned extraction device or extraction method cannot solve the problems existing in the alkaline etching waste liquid extraction and regeneration process.

[0006] In the process of extracting and recycling copper in alkaline etching waste liquid by electrolysis, copper in the alkaline etching waste liquid is recovered by extraction, stripping and electrolysis; the low-copper solution obtained after the etching waste liquid is extracted retains the original chemical components of the etching solution, and after being adjusted, it is used as an etching sub-solution for etching production lines, so that the regeneration and recycling of the alkaline etching waste liquid can be realized. However, the following problems need to be solved in this process: 1. The etching quality of the etching sub-solution decreases after reuse; 2. The impurity content increases after the repeated use of the extraction oil; 3. The oil-water interface is not obvious in the extraction, and the oil-water mixed layer is difficult to eliminate.

[0007] For the problems of etching quality reduction of etching sub-solution and presence of a large amount of impurities in the reused extraction oil, it is because the incomplete extraction in the extraction process leads to mutual residual impurities in the upper layer and the lower layer after the separation; and for the problem of difficulty in eliminating the oil-water mixed layer, under normal circumstances, after the oil and water are fully mixed and left to stand, an emulsion layer will inevitably be formed at the oil-water interface, and the separation speed of the emulsion layer is relatively slow; in addition, the organic impurities with surface activity in the solution will promote the emulsification, and a large amount of stable oil-water emulsion will be dispersed in the alkaline etching waste liquid or the extraction oil, which significantly reduces the extraction efficiency and increases the loss of the extraction oil.

[0008] CN 207680089U discloses an extraction device for processing emulsion layer by using an emulsion layer storage tank, which comprises an extraction kettle, a conductivity meter, an oil phase storage tank, a water phase storage tank, an emulsion layer storage tank and pipelines; the conductivity meter is arranged on the pipeline at the bottom of the extraction kettle, the oil phase storage tank and the water phase storage tank are arranged at the bottom of the extraction kettle and communicate with the bottom of the extraction kettle, and one end of the emulsion layer storage tank directly communicates with the bottom of the extraction kettle without a pump, and the other end communicates with the top of the extraction kettle. However, an external connecting device is still needed to process the emulsion layer, which has a high cost and occupies a large area, and the problem of residual impurities in the upper layer and the lower layer after the extraction separation is not solved.

[0009] Therefore, in view of the deficiencies of the prior art, a reagent for breaking the emulsion layer, accelerating the oil-water separation and avoiding the residual impurities of the extraction oil and the etching sub-solution in the alkaline etching waste liquid extraction process is needed. SUMMARY

[0010] The purpose of the present application is to provide an oil-water separation accelerator for the alkaline etching waste liquid extraction process, which can accelerate the oil-water separation, improve the production efficiency, reduce the loss of the extraction oil and avoid the residual impurities of the extraction oil and the etching sub-solution by designing specific components and contents.

[0011] To achieve the purpose of the present application, the following technical solutions are adopted:

[0012] The application provides an oil-water separation promoter for an alkaline etching waste liquid extraction process, which comprises, in terms of 100wt% of the total mass percentage, 60-90wt% of ethylene glycol monobutyl ether and the balance of nonylphenol polyoxyethylene ether.

[0013] The raw material for the alkaline etching waste liquid extraction process also comprises alkaline etching waste liquid and extraction oil.

[0014] During the extraction or back-extraction process, water and oil can form a milk under the action of stirring. Theoretically, such a milk is unstable, but if there is a surface-active substance in the system, emulsified particles with a double electric layer on the surface will be formed and stably dispersed in the water phase or the oil phase, and the oil-water separation is very slow or even cannot be separated. The oil-water separation promoter provided by the application can destroy the double electric layer on the surface of the emulsified particles by designing specific components and contents, so that the oil particles in the emulsified state are aggregated and separated from the water phase, or the water particles in the emulsified state are aggregated and separated from the oil phase, thereby accelerating the oil-water separation and making the separation more complete, significantly improving the production efficiency, reducing the loss of extraction oil, improving the extraction effect in the extraction process, avoiding the problem of mutual residual impurities between the upper layer liquid and the lower layer liquid after the separation, thereby avoiding the adverse effects of impurities on the reuse of etching sub-liquids, and also without the need to change the existing process equipment, which is simple and convenient to operate.

[0015] The mass percentage of ethylene glycol monobutyl ether in the oil-water separation promoter is 60-90wt%, for example, it can be 60wt%, 70wt%, 75wt%, 80wt% or 90wt%, but is not limited to the listed values, and other values not listed in the value range are also applicable, and preferably 70-80wt%.

[0016] The content of ethylene glycol monobutyl ether and nonylphenol polyoxyethylene ether in the oil-water separation promoter is within a limited range, which can improve the degree of damage of the oil-water separation promoter to the stability of the oil-water emulsion during the alkaline etching waste liquid extraction process, thereby accelerating the oil-water separation and making the oil-water separation more complete.

[0017] Preferably, the oil-water separation promoter further comprises ethanol.

[0018] Preferably, the amount of ethanol is 5-10wt% of the total mass percentage of the oil-water separation promoter, for example, it can be 5wt%, 6wt%, 7wt%, 8wt% or 10wt%, but is not limited to the listed values, and other values not listed in the value range are also applicable, and preferably 6-8wt%.

[0019] The oil-water separation promoter is added with ethanol, so that the components play a synergistic effect, thereby improving the destructiveness of the double electric layer on the surface of the emulsified microparticles, further promoting the aggregation of the oil microparticles in the emulsified state and separating from the water phase, or making the water microparticles in the emulsified state aggregate and separate from the oil phase.

[0020] Preferably, the step of the alkaline etching waste liquid extraction process comprises: uniformly mixing the alkaline etching waste liquid, the extraction oil and the oil-water separation promoter, and then standing to obtain the copper-rich extraction oil and the raffinate.

[0021] After the alkaline etching waste liquid, the extraction oil and the oil-water separation promoter are uniformly mixed, the oil-water separation promoter can accelerate the elimination of the oil-water mixed layer and make the oil-water separation more complete, so that the extraction oil extracts the copper ions in the alkaline etching waste liquid, and finally the copper-rich extraction oil in the upper layer and the raffinate in the lower layer are obtained.

[0022] Preferably, the volume ratio of the extraction oil to the alkaline etching waste liquid is (1.9-2.1):1, which can be 1.9:1, 1.95:1, 2:1, 2.05:1 or 2.1:1, but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0023] Preferably, the components in the alkaline etching waste liquid include NH3·H2O, NH4 + , Cu 2+ and Cl - .

[0024] Preferably, the extraction oil is a mixture of an extractant and an oily solvent.

[0025] Preferably, the oily solvent includes kerosene.

[0026] Preferably, the volume of the oil-water separation promoter is 2-10% of the volume of the extraction oil, which can be 2%, 4%, 6%, 8% or 10%, but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0027] By controlling the ratio of the oil-water separation promoter to the extraction oil, the oil-water separation speed can be effectively promoted and the oil-water separation can be more complete, thereby significantly improving the extraction efficiency, while avoiding the problem of impurities mixed in the extraction oil and the raffinate.

[0028] Compared with the prior art, the present application has the following beneficial effects:

[0029] (1) The oil-water separation accelerator provided by the application can destroy the double electric layer on the surface of emulsified microparticles by designing specific components and contents, so that the oil microparticles in the emulsified state are aggregated and separated from the water phase, or the water microparticles in the emulsified state are aggregated and separated from the oil phase, thereby accelerating the oil-water separation and making the separation more thorough, significantly improving the production efficiency and reducing the loss of extracted oil;

[0030] (2) When the oil-water separation accelerator provided by the application is used in the alkaline etching waste liquid extraction process, the extraction effect in the extraction process can be significantly improved, and a large amount of NH4 + Cl - is avoided in the repeated use of the extraction oil, which further leads to a decrease in extraction capacity. The etching sub-liquid obtained by regenerating the extraction raffinate liquid does not reduce the etching quality after reuse. At the same time, there is no need to change the existing process equipment, and the operation is simple and convenient. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 is a schematic diagram of the copper-rich extraction oil and the raffinate liquid provided by Example 1 of the application;

[0032] Figure 2 is a schematic diagram of the copper-rich extraction oil and the raffinate liquid provided by Comparative Example 3 of the application. DETAILED DESCRIPTION

[0033] The technical solutions of the application will be further described through specific embodiments. Those skilled in the art should understand that the embodiments are only used to help understand the application and should not be regarded as specific limitations on the application.

[0034] Example 1

[0035] The embodiment provides an oil-water separation accelerator for an alkaline etching waste liquid extraction process. The oil-water separation accelerator includes, with the total mass percentage being 100wt%, 75wt% of ethylene glycol monobutyl ether and the balance of nonylphenol polyoxyethylene ether.

[0036] The raw materials used in the alkaline etching waste liquid extraction process also include alkaline etching waste liquid and extraction oil. The steps of the alkaline etching waste liquid extraction process include uniformly mixing the alkaline etching waste liquid, the extraction oil and the oil-water separation accelerator in a measuring cylinder and then standing, to obtain copper-rich extraction oil and raffinate liquid. Figure 1 As shown in the figure, the raffinate liquid is clear and transparent, and no inclusions can be seen. The scale line of the measuring cylinder can be clearly seen.

[0037] The volume ratio of the extraction oil to the alkaline etching waste liquid is 2:1. The components in the alkaline etching waste liquid include NH3·H2O, NH4 + , Cu 2+ and Cl -; the extraction oil is a mixture of N-901 high-efficiency copper extraction agent and kerosene; the volume of the oil-water separation promoter is 6% of the volume of the extraction oil.

[0038] Embodiment 2

[0039] The embodiment provides an oil-water separation promoter for a basic etching waste liquid extraction process, which comprises, in terms of total mass percentage content of 100wt%, 70wt% of ethylene glycol monobutyl ether and the balance of nonylphenol polyoxyethylene ether.

[0040] The raw material for the basic etching waste liquid extraction process also comprises a basic etching waste liquid and an extraction oil; the steps of the basic etching waste liquid extraction process comprise: uniformly mixing the basic etching waste liquid, the extraction oil and the oil-water separation promoter in a measuring cylinder and then standing to obtain copper-rich extraction oil and raffinate.

[0041] The volume ratio of the extraction oil to the basic etching waste liquid is 1.95:1; components in the basic etching waste liquid include NH3·H2O, NH4 + , Cu 2+ and Cl - ; the extraction oil is a mixture of N-901 high-efficiency copper extraction agent and kerosene; the volume of the oil-water separation promoter is 4% of the volume of the extraction oil.

[0042] Embodiment 3

[0043] The embodiment provides an oil-water separation promoter for a basic etching waste liquid extraction process, which comprises, in terms of total mass percentage content of 100wt%, 80wt% of ethylene glycol monobutyl ether and the balance of nonylphenol polyoxyethylene ether.

[0044] The raw material for the basic etching waste liquid extraction process also comprises a basic etching waste liquid and an extraction oil; the steps of the basic etching waste liquid extraction process comprise: uniformly mixing the basic etching waste liquid, the extraction oil and the oil-water separation promoter in a measuring cylinder and then standing to obtain copper-rich extraction oil and raffinate.

[0045] The oil-water volume ratio of the extraction oil to the basic etching waste liquid is 2.05:1; components in the basic etching waste liquid include NH3·H2O, NH4 + , Cu 2+ and Cl - ; the extraction oil is a mixture of N-901 high-efficiency copper extraction agent and kerosene; the volume of the oil-water separation promoter is 8% of the volume of the extraction oil.

[0046] Embodiment 4

[0047] This embodiment provides an oil-water separation accelerator for alkaline etching waste liquid extraction process. Based on a total mass percentage of 100wt%, the oil-water separation accelerator includes: 60wt% ethylene glycol monobutyl ether, with the balance being nonylphenol polyoxyethylene ether.

[0048] The raw materials used in the alkaline etching waste liquid extraction process also include alkaline etching waste liquid and extraction oil; the steps of the alkaline etching waste liquid extraction process include: uniformly mixing alkaline etching waste liquid, extraction oil and oil-water separation promoter in a graduated cylinder and then letting it stand to obtain copper-rich extraction oil and raffinate.

[0049] The oil-to-water volume ratio of the extraction oil to the alkaline etching waste liquid is 1.9:1; the components of the alkaline etching waste liquid include NH3·H2O and NH4+. + Cu 2+ and Cl - The extracted oil is a mixture of N-901 high-efficiency copper extractant and kerosene; the volume of the oil-water separation promoter is 2% of the volume of the extracted oil.

[0050] Example 5

[0051] This embodiment provides an oil-water separation accelerator for alkaline etching waste liquid extraction process. Based on a total mass percentage of 100wt%, the oil-water separation accelerator comprises: 90wt% ethylene glycol monobutyl ether, with the balance being nonylphenol polyoxyethylene ether.

[0052] The raw materials used in the alkaline etching waste liquid extraction process also include alkaline etching waste liquid and extraction oil; the steps of the alkaline etching waste liquid extraction process include: uniformly mixing alkaline etching waste liquid, extraction oil and oil-water separation promoter in a graduated cylinder and then letting it stand to obtain copper-rich extraction oil and raffinate.

[0053] The oil-to-water volume ratio of the extracted oil to the alkaline etching waste liquid is 2.1:1; the components of the alkaline etching waste liquid include NH3·H2O and NH4+. + Cu 2+ And Cl-; the extract oil is a mixture of N-901 high-efficiency copper extractant and kerosene; the volume of the oil-water separation promoter is 10% of the volume of the extract oil.

[0054] Example 6

[0055] This embodiment provides an oil-water separation accelerator for alkaline etching waste liquid extraction process. The difference from Embodiment 1 is that the oil-water separation accelerator also includes ethanol, and the amount of ethanol is 6 wt% of the total mass percentage of the oil-water separation accelerator. The rest are the same as in Embodiment 1.

[0056] Example 7

[0057] The embodiment provides an oil-water separation promoter for an alkaline etching waste liquid extraction process, which is different from the embodiment 1 in that the oil-water separation promoter further comprises ethanol, the amount of the ethanol is 5% of the total mass percentage of the oil-water separation promoter, and the rest is the same as the embodiment 1.

[0058] Embodiment 8

[0059] The embodiment provides an oil-water separation promoter for an alkaline etching waste liquid extraction process, which is different from the embodiment 1 in that the oil-water separation promoter further comprises ethanol, the amount of the ethanol is 10% of the total mass percentage of the oil-water separation promoter, and the rest is the same as the embodiment 1.

[0060] Embodiment 9

[0061] The embodiment provides an oil-water separation promoter for an alkaline etching waste liquid extraction process, which is different from the embodiment 1 in that the oil-water separation promoter further comprises ethanol, the amount of the ethanol is 8% of the total mass percentage of the oil-water separation promoter, and the rest is the same as the embodiment 1.

[0062] Embodiment 10

[0063] The embodiment provides an oil-water separation promoter for an alkaline etching waste liquid extraction process, which is different from the embodiment 1 in that, in addition to adjusting the volume of the oil-water separation promoter to 1% of the volume of the extraction oil, the rest is the same as the embodiment 1.

[0064] Embodiment 11

[0065] The embodiment provides an oil-water separation promoter for an alkaline etching waste liquid extraction process, which is different from the embodiment 1 in that, in addition to adjusting the volume of the oil-water separation promoter to 13% of the volume of the extraction oil, the rest is the same as the embodiment 1.

[0066] Comparative Example 1

[0067] The comparative example provides an oil-water separation promoter for an alkaline etching waste liquid extraction process, which is different from the embodiment 1 in that the mass percentage of the ethylene glycol monobutyl ether in the oil-water separation promoter is adjusted to 50%, and the rest is the same as the embodiment 1.

[0068] Comparative Example 2

[0069] The comparative example provides an oil-water separation promoter for an alkaline etching waste liquid extraction process, which is different from the embodiment 1 in that the mass percentage of the ethylene glycol monobutyl ether in the oil-water separation promoter is adjusted to 95%, and the rest is the same as the embodiment 1.

[0070] Comparative Example 3

[0071] The comparative example provides a solvent for the alkaline etching waste liquid extraction process, the solvent is water, which is different from example 1 in that water is used to replace the oil-water separation promoter in equal volume, and the rest is the same as example 1.

[0072] The schematic diagram of the obtained copper-rich extraction oil and raffinate is shown in Figure 2 As can be seen from the figure, the raffinate is relatively turbid, and the graduated line of the measuring cylinder cannot be clearly seen, indicating that there are impurities in the solution.

[0073] The oil-water separation promoter provided by example 1 and the solvent provided by comparative example 3 are used for the alkaline etching waste liquid extraction process, and the timer is used to count from the beginning of standing. The oil-water separation degree is calculated by the scale of the oil-water boundary line of the copper-rich extraction oil and the raffinate in the measuring cylinder, and the oil-water separation degree at different times is obtained, and the obtained results are shown in Table 1.

[0074] The oil-water separation promoters provided by examples 2-11 and comparative examples 1 and 2 are used for the alkaline etching waste liquid extraction process, and the time required for the oil-water separation degree to reach 100% is measured, as shown in Table 2.

[0075] Table 1

[0076]

[0077] Table 2

[0078]

[0079]

[0080] As can be seen from Table 1 and Table 2, the oil-water separation time can be effectively shortened and the oil-water separation degree can be improved by using the oil-water separation promoter provided by the present application;

[0081] As can be seen from the comparison of example 1 and comparative example 3, without adding the oil-water separation promoter in the extraction process, the oil-water separation time will be significantly prolonged, and the oil-water separation degree will be reduced;

[0082] As can be seen from the comparison of example 1 and examples 2-5 and comparative examples 1 and 2, the content of each component in the oil-water separation promoter is within the preferred range, and the oil-water separation effect is better; exceeding the limited range, the oil-water separation time will be significantly prolonged; as can be seen from the comparison of example 1 and examples 6-9, the addition of ethanol in the oil-water separation promoter is beneficial to the oil-water separation effect; as can be seen from the comparison of example 1 and examples 10 and 11, the volume ratio of the oil-water separation promoter to the extraction oil exceeding the limited range will also adversely affect the oil-water separation effect;

[0083] In summary, the oil-water separation accelerator provided by the present application can destroy the double electric layer on the surface of emulsified microparticles by designing specific components and contents, so that the oil microparticles in the emulsified state are aggregated and separated from the water phase, or the water microparticles in the emulsified state are aggregated and separated from the oil phase, thereby accelerating the oil-water separation and making the separation more thorough, significantly improving the production efficiency, and reducing the loss of extracted oil.

[0084] When the oil-water separation accelerator provided by the present application is used in the alkaline etching waste liquid extraction process, the extraction effect in the extraction process can be significantly improved, and a large amount of NH4 + Further, the etching quality will not be reduced after the etching sub-liquid obtained by regenerating the extraction residue liquid is reused, and the existing process equipment does not need to be changed, and the operation is simple and convenient.

[0085] The above is only a specific embodiment of the present application, but the protection scope of the present application is not limited thereto. It should be understood by those skilled in the art that any changes or replacements within the technical scope disclosed by the present application can be easily thought of by those skilled in the art, and all fall within the protection scope and disclosure scope of the present application.

Claims

1. An oil-water separation accelerator for alkaline etching waste liquid extraction processes, characterized in that, Based on a total mass percentage of 100 wt%, the oil-water separation promoter comprises: 60-90 wt% ethylene glycol monobutyl ether, with the balance being nonylphenol polyoxyethylene ether; The raw materials used in the alkaline etching waste liquid extraction process also include alkaline etching waste liquid and extraction oil.

2. The oil-water separation accelerator according to claim 1, characterized in that, The ethylene glycol monobutyl ether has a mass percentage of 70-80 wt%.

3. An oil-water separation accelerator for alkaline etching waste liquid extraction processes, characterized in that, Based on a total mass percentage of 100 wt%, the oil-water separation promoter comprises: 60-90 wt% ethylene glycol monobutyl ether, 6-8 wt% ethanol, and the balance being nonylphenol polyoxyethylene ether. The raw materials used in the alkaline etching waste liquid extraction process also include alkaline etching waste liquid and extraction oil.

4. The oil-water separation accelerator according to claim 1 or 3, characterized in that, The steps of the alkaline etching waste liquid extraction process include: uniformly mixing alkaline etching waste liquid, extraction oil and oil-water separation promoter and then letting it stand to obtain copper-rich extraction oil and raffinate.

5. The oil-water separation promoter according to claim 4, characterized in that, The volume ratio of the extracted oil to the alkaline etching waste liquid is (1.9-2.1):

1.

6. The oil-water separation promoter according to claim 4, characterized in that, The components in the alkaline etching waste liquid include NH3·H2O and NH4+. + Cu 2+ and Cl - .

7. The oil-water separation promoter according to claim 4, characterized in that, The extraction oil is a mixture of extractant and oily solvent.

8. The oil-water separation accelerator according to claim 7, characterized in that, The oily solvent includes kerosene.

9. The oil-water separation promoter according to claim 4, characterized in that, The volume of the oil-water separation promoter is 2-10% of the extracted oil volume.

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