CN-121971910-A - Method and device for separating and recovering raffinate in vanadium electrolyte production process

CN121971910ACN 121971910 ACN121971910 ACN 121971910ACN-121971910-A

Abstract

The invention discloses a method and a device for separating and recycling raffinate in a vanadium electrolyte production process, wherein the method comprises the steps of S1, inputting the raffinate subjected to pre-degreasing into an adsorption degreasing device for degreasing treatment to obtain regenerated liquid, S2, inputting the regenerated liquid into a vacuum evaporation kettle, S3, carrying out flash evaporation treatment on the regenerated liquid through the vacuum evaporation kettle to obtain ethanol and water mixture steam, S4, separating and recycling the ethanol and water mixture steam through a rectifying tower to obtain ethanol and pure water, and S5, filtering liquid generated in the vacuum evaporation kettle after heating treatment and returning the filtered solid into the raffinate before pre-degreasing, wherein the filtered solid is treated as solid waste. By utilizing the invention, the problem of blockage of the existing raffinate separation and recovery equipment can be solved.

Inventors

SI WENXUE
ZHENG HONGMEI
YANG YONGLIANG
ZHANG SHENGXUE

Assignees

中国恩菲工程技术有限公司
中国有色工程有限公司

Dates

Publication Date: 20260505
Application Date: 20260213

Claims (11)

1. A method for separating and recovering raffinate in the production process of vanadium electrolyte is characterized by comprising the following steps of S1, inputting the raffinate subjected to pre-degreasing into an adsorption degreasing device for degreasing treatment to obtain regenerated liquid; s2, inputting the regenerated liquid into a vacuum evaporation kettle; S3, carrying out flash evaporation treatment on the regenerated liquid through the vacuum evaporation kettle to obtain ethanol and water mixture steam; S4, separating and recycling the ethanol and water mixture steam through a rectifying tower to obtain ethanol and pure water; S5, filtering the liquid generated in the vacuum evaporation kettle, returning the filtered liquid to raffinate before pre-degreasing, and treating the solid generated by filtering as solid waste.
2. The method for separating and recycling the raffinate in the vanadium electrolyte production process according to claim 1, wherein in the step S1, the adsorption degreasing device is used for degreasing the pre-degreased raffinate to obtain a degreased raffinate, and the degreased raffinate is returned to an extraction workshop for recycling, and the adsorption degreasing device adopts a recyclable adsorption column.
3. The method for separating and recovering raffinate in the vanadium electrolyte production process according to claim 2, wherein the adsorption column is disconnected from a raw material raffinate pipeline and an adsorption post-raffinate pipeline after adsorption saturation, and the regeneration liquid in the adsorption column flows into the regeneration liquid tank through a drainage pipeline; cleaning the inside of the adsorption column by pure water, and enabling the formed pure water cleaning liquid to flow into the regeneration liquid tank; the inside of the adsorption column is cleaned by ethanol, and the formed ethanol is cleaned and flows into a regeneration liquid tank; And flushing residual ethanol in the adsorption column to the regeneration liquid tank through water vapor, wherein the flushed adsorption column can be recycled.
4. The method for separating and recycling the raffinate in the production process of the vanadium electrolyte according to claim 1, wherein the raffinate generated in the production process of the vanadium electrolyte is used as a raw raffinate, the temperature of the raw raffinate is 40-50 ℃, and the oil content of the raw raffinate after the pre-degreasing is 20-100 ppm.
5. The method for separating and recovering raffinate from vanadium electrolyte according to claim 1, wherein the oil content of raffinate after oil removal is less than 5ppm.
6. The method for separating and recovering raffinate in a vanadium electrolyte production process according to claim 1, wherein in S2, before inputting the regenerated liquid into a vacuum evaporation tank, further comprising: conveying the regenerated liquid to a regenerated liquid preheater with hot water at 90-100 ℃ through a regenerated liquid conveying pump for preheating; And conveying the regenerated liquid preheated by the regenerated liquid preheater to a vacuum evaporation kettle with a hot water jacket, wherein the hot water temperature of the hot water jacket is 70-90 ℃.
7. The method for separating and recovering raffinate in the vanadium electrolyte production process according to claim 1, wherein in the step S2, the regenerated liquid obtained by cleaning the adsorption degreasing device is conveyed to a vacuum evaporation kettle with a hot water jacket through a regenerated liquid conveying pump, and the hot water temperature of the hot water jacket is 70-90 ℃.
8. The method for separating and recovering raffinate in a vanadium electrolyte production process according to claim 1, wherein in S2, before inputting the regenerated liquid into a vacuum evaporation tank, further comprising: Conveying the regenerated liquid to a regenerated preheater with hot water at 90-100 ℃ for preheating through a regenerated liquid conveying pump; The regenerated liquid preheated by the regenerated liquid preheater is conveyed into a vacuum evaporation kettle without a hot water jacket for flash evaporation treatment, And (3) treating the regenerated liquid subjected to flash evaporation treatment through a residual liquid preheater and a residual liquid circulating pump, and circularly conveying the treated regenerated liquid into the vacuum evaporation kettle without the hot water jacket until ethanol and water mixture steam is obtained.
9. The method for separating and recovering raffinate in a vanadium electrolyte production process according to claim 1, wherein in S4, the separating and recovering process of the ethanol and water mixture vapor by the rectifying tower to obtain ethanol and pure water comprises: The ethanol and water mixture steam is pumped out of the vacuum evaporation kettle through a vacuum pump; Condensing the extracted ethanol and water mixture steam through a condenser; and conveying the condensed ethanol and water mixture steam to a rectifying tower raw material tank, and conveying the ethanol and water mixture steam in the rectifying tower raw material tank to a rectifying tower through a rectifying tower raw material pump.
10. The method for separating and recovering raffinate from vanadium electrolyte according to claim 1, wherein in S4, ethanol formed in the rectifying column is extracted by a rectifying column vacuum pump.
11. The utility model provides a raffinate's separation recovery unit in vanadium electrolyte production process which characterized in that includes: the regenerated liquid obtaining unit is used for inputting the raffinate subjected to the pre-degreasing into the adsorption degreasing device for degreasing treatment to obtain regenerated liquid; the regeneration liquid conveying unit is used for inputting the regeneration liquid into the vacuum evaporation kettle; The vacuum evaporation kettle treatment unit is used for carrying out flash evaporation treatment on the regenerated liquid through the vacuum evaporation kettle to obtain ethanol and water mixture steam; the rectifying tower treatment unit is used for separating and recycling the ethanol and water mixture steam through the rectifying tower to obtain ethanol and pure water; And the residual liquid treatment unit is used for filtering the liquid generated in the vacuum evaporation kettle and returning the filtered liquid to the raffinate before pre-deoiling, and the fixed matters generated by filtering are treated as solid waste.

Description

Method and device for separating and recovering raffinate in vanadium electrolyte production process Technical Field The invention relates to the technical field of raffinate recovery of vanadium-making electrolyte, in particular to a method and a device for separating and recovering raffinate in the production process of vanadium electrolyte. Background The prior methods for preparing the vanadium electrolyte are more, basically wet processes, various extracts and various waste water with similar properties are generated in the process of producing the vanadium electrolyte by the methods, the raffinate is about 100m 3/h per hour in a medium-scale production line, and the raffinate/waste water cannot be directly discharged and needs to be separated and recycled for oil, water and the like. Typically, these raffinates/wastewaters are acidic solutions with ph of about 1, mainly mixtures containing vanadium, chromium, sodium, sulfate, sulfuric acid, water, oil, extractants, which are pre-deoiled, single-stage or multistage adsorbed, the oil content in the raffinates meeting the reuse requirements. There are approximately 2 methods for adsorption degreasing: (1) Resin adsorption is used first, and then activated carbon adsorption is used again. After a period of use, the adsorbent is replaced by a new adsorbent, and the saturated adsorbent is sent to a professional manufacturer for treatment. The adsorbent in the mode cannot be regenerated and recycled on line, is suitable for devices with small production scale, and has the defect that no regenerated liquid needs to be treated, and the adsorbent needs to be replaced periodically. (2) And (3) using a plurality of resin adsorption columns, adsorbing 1 or more resin adsorption columns, standing by 1 or more resin adsorption columns, switching periodically, and regenerating the adsorbed adsorbent again for later use. The adsorbent in the mode can be regenerated and recycled on line, is suitable for devices with large production scale, can generate regenerated liquid to be treated, does not need to be replaced periodically, and has low operation cost. With the increase in the size of the apparatus, the (2) mode is generally adopted. The oil adsorbed by the adsorbent is washed by water, then the adsorbent is washed by ethanol, the oil adsorbed by the adsorbent is resolved, and finally the ethanol in the adsorbent is completely washed by steam. In the process, the feed liquid generated by water washing can be returned to an adsorption feed tank, the ethanol flushing feed liquid and the steam flushing feed liquid are collected and are called regeneration liquid, and the regeneration liquid is sent to an ethanol, water and oil separation recovery device. If the regenerated liquid is directly sent into a rectifying tower, along with the evaporation of ethanol and water, vanadium, chromium and sodium salt are crystallized and separated out in a stripping section and a tower kettle, and are mixed with oil to form greasy dirt with very poor fluidity, and the greasy dirt is attached to pipelines, valves and tower internals, so that the rectifying tower cannot operate due to final blockage. In order to solve the problem of equipment blockage, a new ethanol, water and oil recovery method is needed. Disclosure of Invention In view of the above problems, the present invention aims to provide a method and a device for separating and recovering raffinate in a vanadium electrolyte production process, so as to solve the problem of blockage of the existing separating and recovering equipment for raffinate. The invention provides a method for separating and recovering raffinate in the production process of vanadium electrolyte, which comprises the following steps of, S1, inputting the pre-deoiled raffinate into an adsorption deoiling device for deoiling treatment to obtain regenerated liquid; s2, inputting the regenerated liquid into a vacuum evaporation kettle; S3, carrying out flash evaporation treatment on the regenerated liquid through the vacuum evaporation kettle to obtain ethanol and water mixture steam; S4, separating and recycling the ethanol and water mixture steam through a rectifying tower to obtain ethanol and pure water; S5, filtering the liquid generated in the vacuum evaporation kettle, returning the filtered liquid to raffinate before pre-degreasing, and treating the solid generated by filtering as solid waste. In addition, in the S1, the adsorption degreasing device is used for degreasing the pre-degreased raffinate to obtain a degreased raffinate, and returning the degreased raffinate to an extraction workshop for recycling, wherein the adsorption degreasing device adopts a recyclable adsorption column. In addition, the optional structure is that the adsorption degreasing device adopts a recyclable adsorption column. In addition, the selective structure is that the adsorption column is disconnected with a raw material raffinate pipeline and an adsorption back raffi