Method for collecting rare earths from a solution or organic phase of waste water

Abstract

The application discloses a method for collecting organic phase in rare earth material liquid or wastewater, comprising the following steps: taking the rare earth material liquid or wastewater containing organic phase generated in the rare earth production process as a treatment object, analyzing the oil content of the treatment object, determining the phase ratio of the treatment object according to the oil content, adding kerosene as a collector into the treatment object according to the determined phase ratio, collecting the organic phase in the treatment object, separating the phases by using a separating funnel, separating out the water phase, and recycling the organic phase. The application can collect the organic phase in the rare earth material liquid or wastewater containing organic phase generated in the rare earth smelting and separation process, and reduce the oil content of the rare earth material liquid and the wastewater.

Description

Technical Field

[0001] This invention belongs to the field of hydrometallurgy, specifically, it relates to a method for collecting the organic phase from rare earth slurry or wastewater. Background Technology

[0002] During the rare earth smelting and separation process, the rare earth slurry and saponification wastewater produced by the extraction and separation process inevitably carry or dissolve some organic phases, thus generating rare earth slurry and wastewater containing organic matter.

[0003] CN202311802891.8 discloses a method for recovering the organic phase in raffinate. The method involves generating a large amount of foam using a vertical tube bubble generator to bring the organic phase in the raffinate to the solution surface. The organic phase is then recovered through methods such as oil skimming and adsorption of oil-absorbing substances in a connecting pipe, thereby reducing the organic phase content in the raffinate.

[0004] The paper, "Removal or Recovery of Oil from Raffinate and Back-extraction Liquid," takes P204 extraction of manganese as an example. It explores that the oil components in raffinate and back-extraction liquid may include P204 extractant, saponified P204, metal extracts and their various hydrolysis products, and sulfonated kerosene. During the solvent extraction process for recovering valuable metals such as nickel, cobalt, and manganese from waste lithium-ion battery cathode materials, the organic matter carried in the raffinate and back-extraction liquid leads to significant extractant loss. The paper, "Production Practice of Oil Removal and Recovery of Extracted Organic Phase in Extractive Metallurgy Process," studied a multi-stage coalesced core modified material oil separator designed and used by a domestic enterprise. During use, the primary oil removal rate did not meet the design requirements. After analyzing the reasons, a combination device of dissolved air pump and air flotation clarification tank was added, and an activated carbon adsorption tank security filter device was added at the end of the oil separator. The oil removal rate met the design requirements, and the average oil content of the solution after oil removal was less than 10 mg / L.

[0005] Currently, the main methods for recovering the organic phase of the raffinate are dissolved air flotation, adsorption, and coagulation, which are difficult to deeply recover the organic phase. For the organic phase in rare earth feed liquid and wastewater, it is even more difficult to recover and reuse it. Summary of the Invention

[0006] The purpose of this invention is to provide a method for capturing the organic phase in rare earth slurry or wastewater, which can capture the organic phase in rare earth slurry or wastewater containing organic phase generated during rare earth smelting and separation, thereby reducing the oil content of rare earth slurry and wastewater.

[0007] To achieve the above objectives, the technical solution used in this invention is: Methods for collecting the organic phase from rare earth slurry or wastewater include: Using rare earth slurry or wastewater containing organic phase generated during rare earth production as the treatment object, the oil content of the treatment object is analyzed, and the ratio of the treatment object is determined based on the oil content. According to the determined ratio, kerosene is used as a collector and added to the object to be treated to collect the organic phase in the object to be treated. Use a separatory funnel to separate the aqueous phase and recover the organic phase.

[0008] Furthermore, the ratio of kerosene to wastewater is 1:1 to 1:30, and the ratio of kerosene to rare earth feed liquid is 1:1 to 1:30.

[0009] Furthermore, using the ratio as a control condition, kerosene is added to the treatment object containing the organic phase according to the ratio. After stirring, the organic phase in the treatment object is fully mixed and collected. Stirring for 5-60 minutes allows the organic phase entrained in the kerosene and water phase to dissolve, thereby achieving the purpose of collecting the organic phase.

[0010] Furthermore, an intermittent collection method is adopted. After the target substance is mixed and reacted with the collector in the reaction tank for a certain period of time, the aqueous phase is separated, and the collector remains in the reaction tank. The target substance is then added to the reaction tank again to continue the collection and mixing reaction. After a certain period of reaction, the aqueous phase is separated, and the collector remains in the reaction tank. This process is repeated multiple times until the collector is saturated, at which point a new collector is replaced.

[0011] Furthermore, a continuous multi-stage countercurrent or cocurrent collection method is adopted. After the target substance is mixed and reacted with the collector in the reaction tank for a certain period of time through multi-stage countercurrent or cocurrent, the aqueous phase is separated out, and the collector is recycled until the collector is saturated, at which point a new collector is replaced.

[0012] The technical effects of this invention include: This invention involves the organic phase capture of rare earth slurry or wastewater containing organic phase generated during rare earth smelting and separation, thereby reducing the oil content of rare earth slurry and wastewater. The recovered organic phase can be reused after treatment.

[0013] 1. Organic phase capture is performed on organic rare earth feed solutions and organic wastewater, significantly reducing the oil content in rare earth feed solutions and wastewater.

[0014] Rare earth feed solutions and wastewater containing organic phases are generated during rare earth extraction and separation processes by the entrainment and miscibility of certain organic phases, mainly containing extractants and sulfonated kerosene. This application utilizes the principle of "like dissolves like" to recover the entrained and miscible organic phases by adding kerosene to the rare earth feed solutions and wastewater in a specific ratio. This reduces the loss of extractants during rare earth production, achieving the recovery of high-value organics and reducing organic consumption per unit. Simultaneously, it minimizes the impact of residual organics in the solution on product quality and subsequent process control.

[0015] 2. A physical oil removal and recovery method is adopted. Kerosene is added to capture the organic phase using the principle of "like dissolves like". This will not affect the quality of the organic phase. The recovered organic phase can be reused in production as a production reagent, thereby reducing the unit consumption of production.

[0016] 3. Its application in the field of rare earth smelting and separation has created good environmental and economic benefits.

[0017] The entire process is simple, convenient, quick, and economical, while reducing environmental pollution and improving environmental quality. Its application in rare earth smelting and separation has generated significant environmental and economic benefits, and it has broad prospects for future application and development in the field of hydrometallurgy. Attached Figure Description

[0018] Figure 1 This is a process flow diagram of the method for collecting the organic phase in rare earth liquid or wastewater in this invention. Detailed Implementation

[0019] The following description fully illustrates specific embodiments of the present invention to enable those skilled in the art to practice and reproduce it. To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0020] like Figure 1 The diagram shown is a process flow chart of the method for collecting the organic phase in rare earth liquid or wastewater according to the present invention.

[0021] The specific steps for collecting the organic phase from rare earth slurry or wastewater are as follows: Step 1: Take the rare earth liquid or wastewater containing organic phase generated during the rare earth production process as the treatment object, analyze the oil content of the treatment object, and determine the ratio of the treatment object based on the oil content; The ratio of kerosene to wastewater is 1:1 to 1:30, and the ratio of kerosene to feed liquid is 1:1 to 1:30.

[0022] The ratio of the organic phase (O) to the aqueous phase (A) is expressed as O / A. Sometimes the reciprocal of the ratio is called the "water-oil ratio". If the extraction process is continuous, the ratio can also be expressed as the volume ratio of the organic phase and the aqueous phase flowing per minute, i.e., the ratio equals the flow rate ratio.

[0023] Step 2: According to the determined ratio, kerosene is added as a collector to the object to be treated to collect the organic phase in the object to be treated; This application utilizes the principle of "like dissolves like" to achieve organic phase capture. Kerosene is added to rare earth slurry and wastewater containing organic phase at a certain ratio. After stirring for 5-60 minutes, the organic phase in the target material is fully mixed. The kerosene and the organic phase entrained in the aqueous phase are mutually soluble, thus achieving the purpose of capturing the organic phase.

[0024] Kerosene is used to capture the organic phase in rare earth feed solutions / wastewater containing organic rare earths: using the ratio as a control condition, kerosene is added to rare earth feed solutions or wastewater containing organic phases according to a certain ratio.

[0025] Step 3: Use a separatory funnel to separate the aqueous phase and recover the organic phase.

[0026] Intermittent collection can be used. After the feed liquid or wastewater is mixed with the collector in the reaction tank for a certain period of time, the aqueous phase is separated and the collector remains in the reaction tank. Feed liquid or wastewater is added to the reaction tank again to continue the collection and mixing reaction. After a certain period of reaction, the aqueous phase is separated and the collector remains in the reaction tank. This process is repeated several times until the collector is saturated and no longer has the ability to collect. Then, a new collector is replaced.

[0027] Alternatively, a continuous multi-stage countercurrent or cocurrent collection method can be adopted. After the feed liquid or wastewater is mixed and reacted with the collector in the reaction tank for a certain period of time through multi-stage countercurrent or cocurrent, the aqueous phase is separated out. The collector can be recycled until it is saturated and no longer has the ability to collect, at which point a new collector is replaced.

[0028] After the kerosene recovery process, the oil content of the treated rare earth slurry and wastewater is significantly reduced, and the recovered organic phase can be reused in the production process after further treatment. This method is simple to control, highly efficient, economical, and suitable for industrial production applications.

[0029] Example 1 The oil content in the rare earth feed solution was analyzed, and the data are shown in Table 1 below.

[0030] Table 1. Rare Earth Feed Liquid Oil Content

[0031] Kerosene collection from rare earth feed solution containing organic rare earth: Add 35-1000 mL of kerosene to 1000 mL of rare earth feed solution, stir for 5-60 minutes, separate the phases using a separatory funnel, and analyze the oil content in the rare earth feed solution. Repeat the above steps four times. The data are shown in Table 2 below.

[0032] Table 2. Rare earth liquid oil content after kerosene harvesting

[0033] Example 2 The oil content data in the rare earth feed solution are shown in Table 3 below.

[0034] Table 3. Rare Earth Feed Liquid Oil Content

[0035] Kerosene collection from rare earth feed solution containing organic rare earth: Add 35-1000 mL of kerosene to 1000 mL of rare earth feed solution, stir for 5-60 minutes, separate the phases using a separatory funnel, and analyze the oil content in the rare earth feed solution. Repeat the above steps four times. The data are shown in Table 4 below.

[0036] Table 4. Rare earth liquid oil content after kerosene harvesting

[0037] Example 3 (1) The oil content in the wastewater was analyzed, and the data are shown in Table 5 below. Table 5 Oil content in wastewater

[0038] (2) Wastewater kerosene collection: Add 35-1000mL of kerosene to 1000mL of wastewater, stir for 5-60 minutes, separate the phases using a separatory funnel, and analyze the oil content of the wastewater. Repeat the above steps four times. The data are shown in Table 6 below.

[0039] Table 6 Oil content in wastewater after kerosene collection

[0040] The terminology used in this invention is descriptive and exemplary, not restrictive. Since this invention can be embodied in many forms without departing from the spirit or essence of the technical solution, it should be understood that the above embodiments are not limited to any of the foregoing details, but should be interpreted broadly within the spirit and scope defined by the appended claims. Therefore, all variations and modifications falling within the scope of the claims or their equivalents should be covered by the appended claims.

Claims

1. A method for collecting the organic phase from rare earth liquid or wastewater, characterized in that, include: Using rare earth slurry or wastewater containing organic phase generated during rare earth production as the treatment object, the oil content of the treatment object is analyzed, and the ratio of the treatment object is determined based on the oil content. According to the determined ratio, kerosene is used as a collector and added to the object to be treated to collect the organic phase in the object to be treated. Use a separatory funnel to separate the aqueous phase and recover the organic phase.

2. The method for collecting the organic phase from rare earth slurry or wastewater as described in claim 1, characterized in that, The ratio of kerosene to wastewater is 1:1 to 1:30, and the ratio of kerosene to rare earth feed liquid is 1:1 to 1:

30.

3. The method for collecting the organic phase from rare earth slurry or wastewater as described in claim 1, characterized in that, Using the ratio as a control condition, kerosene is added to the treatment object containing the organic phase according to the ratio. After stirring, the organic phase in the treatment object is fully mixed and collected. Stirring for 5-60 minutes allows the organic phase entrained in the kerosene and water phase to dissolve, thus achieving the purpose of collecting the organic phase.

4. The method for collecting the organic phase from rare earth slurry or wastewater as described in claim 1, characterized in that, An intermittent collection method is adopted. After the target substance is mixed and reacted with the collector in the reaction tank for a certain period of time, the aqueous phase is separated and the collector remains in the reaction tank. The target substance is then added to the reaction tank again to continue the collection and mixing reaction. After a certain period of reaction, the aqueous phase is separated and the collector remains in the reaction tank. This cycle is repeated multiple times until the collector is saturated, at which point a new collector is replaced.

5. The method for collecting the organic phase from rare earth slurry or wastewater as described in claim 1, characterized in that, The collection method employs a continuous multi-stage countercurrent or cocurrent flow. After the target substance reacts with the collector in the reaction tank for a certain period of time through multi-stage countercurrent or cocurrent flow, the aqueous phase is separated out, and the collector is recycled until the collector is saturated, at which point a new collector is replaced.

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