CN114380435B - Online recovery process for lost organic phase of hydrometallurgical extraction separation system - Google Patents
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Abstract
The invention provides an on-line recovery process of a lost organic phase of a hydrometallurgical extraction separation system, which comprises a recovery process of the lost organic phase of a product water phase, a recovery process of the lost organic phase of a waste water phase and a recovery process of the lost organic phase in acid mist waste gas; and (3) allowing the water phase to enter a fiber ball adsorption tower and an activated carbon adsorption tower to adsorb organic matters in the water phase, and when the water phase needs to be regenerated after the adsorption is finished, performing supercritical carbon dioxide extraction to regenerate the fiber balls and the activated carbon and recovering the adsorbed organic matters. The invention adopts an on-line recovery process in the main organic phase loss link of the hydrometallurgy extraction and separation system, not only ensures the purity of the product, removes water pollution and atmospheric pollution, recovers the extractant, avoids frequent replacement of the adsorption material, ensures more stable and environment-friendly production process, and obviously improves the production efficiency. The invention adopts supercritical carbon dioxide extraction technology, so that the recovered organic matters are not subjected to chemical change and can be completely returned to the system for reuse.
Description
Technical Field
The invention belongs to the technical field of hydrometallurgy, relates to an extraction separation system, and in particular relates to an on-line recovery process of an organic phase lost by the hydrometallurgy extraction separation system.
Background
Hydrometallurgy is an independent technology which is a metallurgical technology developed rapidly during the world war II, and because the traditional pyrometallurgy cannot be adopted when extracting some mineral substances such as uranium and the like, the separation and purification can only be carried out in chemical solution, and the method for extracting metals is hydrometallurgy. In recent decades, with the development of rare earth and nonferrous metal industries, the requirements of people on the purity and the accurate proportioning of materials are higher and higher, the separation technology of similar metals is developed very rapidly, and particularly, the extraction separation technology is utilized to ensure that the purity of the metals is higher, and the proportioning of alloy materials is more accurate, so that more excellent new materials such as corrosion-resistant and high-temperature-resistant alloy, power battery anode materials and the like are produced. However, during the hydrometallurgical extraction separation process, a significant portion of the organic extractant runs off with the aqueous phase, which increases production costs and affects product quality and also causes environmental pollution. The lost organic phase mainly goes to three aspects, namely, the lost organic phase is lost along with the product phase, the product is dissolved in water in the form of a certain salt such as sulfate after separation, then the next procedure is carried out, the organic matters emulsified and dissolved in the product solution are usually demulsified and removed, and then the deoiling material such as fiber balls are used for adsorbing a part of the organic phase emulsified and dissolved in the water phase, and then a large amount of activated carbon is used for adsorption for advanced treatment; on the other hand, along with the organic phase lost by the wastewater, the part of the wastewater is high-salt wastewater with the salt content of more than 5 percent, such as sodium sulfate-containing wastewater, and the COD (chemical oxygen demand) is generally higher than 2000mg/L, and the total amount of the lost organic phase is considerable due to the relatively large amount of the wastewater in the extraction section although the concentration of the lost organic matters in the wastewater is not high; the third aspect is that as the acid mist volatilizes the organic phase, because the extraction is usually carried out repeatedly at a certain temperature to selectively distribute metal ions in the aqueous phase and the organic phase, which can generate acid mist, the current mature extraction equipment is a polyvinyl chloride plastic tank, and absolute sealing is not possible, so that the acid mist in the extraction tank needs to be led out of the system organically in order to improve the operation environment, and thus, part of the solvent volatilizes to pollute VOCs (volatile organic compounds).
The organic phase lost during the extraction process is not effectively recovered by the production unit, and in fact, is still a good raw material, but is only dissolved in the aqueous phase or volatilized, and the production unit takes some methods to treat the organic phase as impurities, wastes and pollutants in consideration of the quality of the product and the pressure of environmental protection, which leads to the loss of expensive extractant, more importantly, the waste treatment is time-consuming and labor-consuming and generates new pollution, and in fact, converts one pollution form into another environment-friendly acceptable form.
The series of problems finally lead to a large amount of loss of an extracted organic phase, low product purity, high wastewater treatment difficulty, large waste residue amount, difficult disposal of waste salt, difficult complete automation of the whole process, high labor intensity of workers, low production efficiency and high cost, and have severely restricted the improvement of hydrometallurgical productivity and the modernization of production. To solve these problems, a number of improvements have been made by those skilled in the hydrometallurgical arts.
Wu Qingyan in the proposal of analysis and prevention of pollution sources of hydrometallurgy of nickel and cobalt (J, nonferrous metals of the world, 2019, 3 months, P4-8) the current organic phase loss and corresponding disposal method of the extraction section of hydrometallurgy industry are systematically introduced, the emulsified organic phase is generally recovered as much as possible by adopting methods such as demulsification phase separation, fiber ball adsorption and the like, but the volatile organic matters and the organic matters dissolved in the water phase (product phase and waste water phase) are treated as pollutants by using active carbon adsorption or other methods for oxidative decomposition of the organic matters, so that the aim of reducing COD and VOCs is achieved.
The application numbers of the Chinese patents CN201910255859.X, CN201811419673.5, CN201810909767.4, CN201510684466.2 and the like disclose hydrometallurgical wastewater treatment methods, which are mainly characterized in that organic matters dissolved in high-salt wastewater are oxidized and decomposed by means of electrocatalytic oxidation, ozone oxidation, hydrogen peroxide oxidation and the like, even the organic matters are oxidized and then are deeply treated by activated carbon adsorption, so that COD in the water is reduced for preparing for the next desalination, but the methods are not industrially adopted except for the hydrogen peroxide oxidation method, the main reasons are that the efficiency of removing the organic matters in the water is not high, the operation cost is too high, and the phosphoric acid generated by oxidizing an extractant containing phosphate is easy to be adhered to a heat exchanger to influence the subsequent desalination treatment by trace calcium phosphate contained in the wastewater, and in addition, the replaced activated carbon belongs to unit treatment of hazardous waste which is required to be qualified.
The application numbers of CN201820163953.3, CN201810091845.4 and other Chinese patents disclose a wet metallurgy extraction section oily acid mist treatment process, which mainly adopts alkaline water absorption and neutralization and then oil-water separation, and the method has better acid mist treatment effect, but is not ideal for volatile oil treatment, so that the aim of treating VOCs can not be achieved, and in addition, COD in absorption wastewater is increased, VOCs pollution is changed into water pollution, and the treatment cost is increased.
In the prior art, the hydrometallurgical extraction separation process cannot realize the whole process continuity, the organic impurities in the online treatment products are high, the COD in the wastewater is high, and the production cost and quality of the products are affected by exceeding of VOCs in acid mist.
By analyzing the prior reported technology, the methods in the prior art have a misarea, namely, organic phases emulsified and dissolved in an aqueous phase or volatilized along with acid mist are regarded as impurities and wastes to be abandoned and recycled, the starting point is mised, the treatment method is not ideal, and in fact, the organic phases are still good raw materials, and if the organic phases can be effectively recycled and returned to a system for reuse, not only the production cost is reduced, but also the pollution problem is solved.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide an on-line recovery process for the lost organic phase of a hydrometallurgical extraction separation system, which solves the technical problem that the organic phase is not recovered in the hydrometallurgical extraction separation process in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
an on-line recovery process of a lost organic phase of a hydrometallurgical extraction separation system comprises a recovery process of the lost organic phase of a product water phase, a recovery process of the lost organic phase of a wastewater phase and a recovery process of the lost organic phase in acid mist waste gas;
the recovery process of the lost organic phase in the product water phase is the same as that of the lost organic phase in the wastewater phase, and a product water phase or wastewater phase lost organic phase recovery sub-device is adopted;
the organic phase recovery sub-device for the product water phase or the wastewater phase loss comprises a temporary storage tank which is connected with a pipeline of the product water phase or the wastewater phase in the hydrometallurgical extraction separation system, the temporary storage tank is connected with a liquid inlet of an ultrasonic demulsifier through a water pump, a liquid outlet of the ultrasonic demulsifier is connected with a feed inlet of a super-oleophobic hydrophilic membrane separator, an organic phase outlet at the upper end of the super-oleophobic hydrophilic membrane separator is connected with an organic phase collecting tank, a water phase outlet at the lower end of the super-oleophobic hydrophilic membrane separator is connected with a bottom valve of a fiber ball adsorption tower, a discharge port at the upper end of the fiber ball adsorption tower is connected with a bottom valve of a first activated carbon adsorption tower, and a discharge port at the upper end of the first activated carbon adsorption tower is connected with a pipeline of the next procedure in the hydrometallurgical extraction separation system;
the fiber ball adsorption tower and the upper end inlet of the first activated carbon adsorption tower are respectively connected with a first liquid carbon dioxide pipeline with a first flowmeter; the bottom valve of the fiber ball adsorption tower is connected with a first organic matter recovery tank, and the bottom valve of the first activated carbon adsorption tower is connected with a second organic matter recovery tank;
after a product water phase or wastewater phase enters a temporary storage tank, the product water phase or wastewater phase is sent into an ultrasonic demulsifier through a water pump to carry out demulsification, then the product water phase or wastewater phase enters a super oleophobic hydrophilic membrane separator to carry out separation of an organic phase and a water phase, the organic phase enters an organic phase collecting tank, the water phase enters a fiber ball adsorption tower and a first activated carbon adsorption tower to adsorb organic matters in the water phase, and the water phase after passing through the first activated carbon adsorption tower enters the next working procedure in a hydrometallurgical extraction separation system;
when regeneration is needed after adsorption is completed, introducing liquid carbon dioxide into the fiber ball adsorption tower and the first activated carbon adsorption tower, regulating the liquid carbon dioxide to a supercritical state in the fiber ball adsorption tower and the first activated carbon adsorption tower, and extracting organic matters adsorbed in the fiber ball adsorption tower and the first activated carbon adsorption tower by using carbon dioxide supercritical extraction so that the fiber balls in the fiber ball adsorption tower and the activated carbon in the first activated carbon adsorption tower are regenerated, and enabling the organic matters obtained by extraction to enter a first organic matter recovery tank and a second organic matter recovery tank;
the recovery process of the lost organic phase in the acid mist waste gas adopts a recovery sub-device of the lost organic phase in the acid mist waste gas;
the organic phase recovery sub-device for the acid mist waste gas loss comprises a second active carbon adsorption tower, wherein a bottom valve of the second active carbon adsorption tower is connected with a pipeline of the acid mist waste gas in an induced air system in a hydrometallurgical extraction separation system, and a discharge port at the upper end of the second active carbon adsorption tower is connected with a pipeline of an acid mist absorption procedure in the hydrometallurgical extraction separation system;
the inlet at the upper end of the second activated carbon adsorption tower is connected with a second liquid carbon dioxide pipeline with a second flowmeter; the bottom valve of the second activated carbon adsorption tower is connected with a third organic matter recovery tank;
the acid mist waste gas enters a second activated carbon adsorption tower to adsorb organic matters in the acid mist waste gas, and the acid mist waste gas after passing through the second activated carbon adsorption tower enters an acid mist absorption procedure in a hydrometallurgical extraction separation system;
when regeneration is needed after the adsorption is finished, introducing liquid carbon dioxide into the second activated carbon adsorption tower, regulating the liquid carbon dioxide to a supercritical state in the second activated carbon adsorption tower, and performing supercritical carbon dioxide extraction on organic matters adsorbed in the second activated carbon adsorption tower to regenerate the activated carbon in the second activated carbon adsorption tower, wherein the organic matters obtained by extraction enter a third organic matter recovery tank.
The invention also has the following technical characteristics:
the ultrasonic demulsification process conditions in the ultrasonic demulsifier are as follows: the ultrasonic frequency is 20-25 KHz, the residence time of the product water phase or waste water phase in the ultrasonic demulsifier is less than 15min, and the flow rate of the product water phase or waste water phase and the position of the overflow port of the product water phase or waste water phase are controlled.
The aperture of the super oleophobic hydrophilic membrane in the super oleophobic hydrophilic membrane separator is 0.5-15 microns.
The technological conditions of supercritical carbon dioxide extraction and regeneration are as follows: the pressure is 7.39-15.9 Mpa, the temperature is 31.1-65 ℃, and the supercritical carbon dioxide extraction residence time is 15-180 min.
And a return pipe is arranged between the ultrasonic demulsifier and the temporary storage tank.
The fiber ball adsorption tower and the upper inlet of the first activated carbon adsorption tower are also respectively communicated with the first gaseous carbon dioxide pipeline.
The fiber ball adsorption tower, the first activated carbon adsorption tower and the second activated carbon adsorption tower are all arranged in parallel, one by one and two.
The inlet at the upper end of the second activated carbon adsorption tower is also connected with a second gaseous carbon dioxide pipeline.
The fiber ball adsorption tower, the first active carbon adsorption tower, the second active carbon adsorption tower, the first organic matter recovery tank, the second organic matter recovery tank and the third organic matter recovery tank are respectively provided with a temperature control jacket, a thermometer, a pressure gauge, a safety valve and/or a blow-off valve, and a heating belt is arranged behind the blow-off valve.
Compared with the prior art, the invention has the following technical effects:
the invention adopts an on-line recovery process in the main organic phase lost links (product water phase, raffinate, saponification wastewater and acid mist system) of the hydrometallurgical extraction and separation system, thereby not only ensuring the purity of the product, removing water pollution and atmospheric pollution, recovering the extractant, avoiding frequent replacement of the adsorption material, ensuring the production process to be more stable and environment-friendly, and obviously improving the production efficiency.
And (II) the invention adopts ultrasonic demulsification and super oleophobic hydrophilic membrane separation technology to fully separate emulsified and insoluble organic phases, thereby reducing the pressure and saturation frequency of an adsorption link, and compared with the traditional separation technology by utilizing specific gravity difference, the super oleophobic hydrophilic membrane separation technology is more thorough and is not influenced by an oil-water interface.
And (III) the invention adopts supercritical carbon dioxide extraction technology, so that the recovered organic matters are not subjected to chemical change and can be completely returned to the system for reuse.
And (IV) the organic phase is thoroughly recovered, so that the quality of the product is better, and COD and VOCs in the wastewater and the waste gas directly meet the requirements of the next procedure.
And (V) the regeneration effect of the supercritical carbon dioxide on the adsorption material fiber balls and the activated carbon is superior to that of other regeneration technologies.
Drawings
FIG. 1 is a schematic diagram of the structure of a device for recovering lost organic phase in the aqueous or wastewater phase of the product of the present invention.
Fig. 2 is a schematic structural diagram of a device for recovering lost organic phase in acid mist waste gas.
The meaning of each reference numeral in the figures is: 1-a product water phase or wastewater phase loss organic phase recovery sub-device, 2-an acid mist waste gas loss organic phase recovery sub-device, 3-a product water phase or wastewater phase pipeline, 4-a next process pipeline, 5-an acid mist waste gas pipeline in an induced air system and 6-an acid mist absorption process pipeline;
101-temporary storage tanks, 102-water pumps, 103-ultrasonic demulsifiers, 104-super oleophobic hydrophilic membrane separators, 105-organic phase collecting tanks, 106-fiber ball adsorption towers, 107-first activated carbon adsorption towers, 108-first flowmeters, 109-first liquid carbon dioxide pipelines, 110-first organic matter recovery tanks, 111-second organic matter recovery tanks, 112-return pipes and 113-first gaseous carbon dioxide pipelines;
201-a second activated carbon adsorption tower, 202-a second flowmeter, 203-a second liquid carbon dioxide pipeline, 204-a third organic matter recovery tank, 205-a second gaseous carbon dioxide pipeline.
The following examples illustrate the invention in further detail.
Detailed Description
From the above background analysis, the organic phase flow loss of the hydrometallurgical extraction section has three main aspects. The organic phase which runs off along with the water phase of the product enters the product, thus the quality of the product is necessarily affected, the organic phase can only be treated by a physical method which does not produce secondary pollution on the product, the oil-absorbing resin such as fiber balls and activated carbon are successfully used for combined adsorption in industry to achieve the aim of removing organic impurities, but the regeneration process of the oil-absorbing resin is complex, the replaced resin is generally regenerated by a distillation method and the like, the waste activated carbon is used as waste to be treated as a qualification unit, the waste is labor-and time-consuming, the cost is high, and the problem of recovering the lost organic phase is not fundamentally solved. The organic phase lost with the wastewater is mainly dissolved organic matters, because the pH value of the wastewater is generally close to neutrality, the phosphate extractant is dissolved in the water in the form of sodium salt, the extractant cannot be recovered through oil-water separation, the concentration is relatively low, the wastewater amount is relatively large, the production unit generally treats the wastewater as waste, but the high-salt wastewater cannot be treated through a low-cost method such as biochemistry and the like, and can only be treated through an oxidative decomposition method such as electrochemical oxidation, ozone oxidation, hydrogen peroxide oxidation and the like, so that the treatment cost is greatly increased, and in fact, if the pH value of the wastewater is adjusted to about 3.5, the effect of adsorbing the organic matters in the wastewater by using the activated carbon is very good, and like removing the organic matters in the product, COD can be reduced to below 50mg/L from a few kilomg/L, because the extractant is reduced to an original state from the sodium salt state when the pH value is equal to 3.5, the adsorption efficiency of the activated carbon can reach more than 98%, but the treatment cost is relatively high because the amount of the waste activated carbon generated by the method is relatively large, and the production unit is undesirable. The organic volatile along with the acid mist is mainly solvent kerosene, only part of kerosene can be condensed by an alkali liquor absorption method for treating the acid mist, and part of VOCs still cannot reach the standard, and COD in the absorbed water exceeds the standard, so that the conventional method is to firstly absorb volatile oil by using activated carbon and then absorb the acid mist by using alkaline water, and the waste activated carbon is difficult to regenerate by using methods such as steam heating and the like due to higher boiling point of the absorbed kerosene and can only be abandoned.
From the analysis, the organic phase adsorption fiber balls and the activated carbon which are lost in the three aspects can be adsorbed to meet the requirements of product quality and environmental protection, but the adsorption capacity of the adsorption fiber balls and the activated carbon is limited, so that the adsorption fiber balls and the activated carbon are required to be replaced after being saturated and invalid soon, and the disposal of the replaced adsorption fiber balls and the activated carbon is also a problem. The organic matters which are actually dispersed and dissolved in the water phase mainly have two states, one is oil drops with different particle sizes which are emulsified in the water phase; the other is an organic substance dissolved in the aqueous phase. The emulsified organic matters are demulsified and split-phase to recover part of the organic matters in the water as far as possible, so that the replacement frequency of the adsorption fiber balls and the activated carbon is reduced, and the adsorption saturated fiber balls and the activated carbon are regenerated, especially on-line regeneration, and meanwhile, the lost organic matters are recovered, so that the key of solving the problem is realized. As for the emulsified organic phase, the common demulsification methods include an ultrasonic method, an air floatation method and a chemical demulsifier, the methods are the most concise and have no secondary pollution, but the ultrasonic wave is not absolute, and the method can not only demulsifie but also accelerate the emulsification, so that the frequency and the residence time are generally controlled to only gather small oil drops into large oil drops, and then a part of the organic phase is separated by utilizing the specific gravity difference, but the separation is not very thorough, and the oil-water interface is not well judged. Regarding regeneration of the adsorbent fiber balls, the data show that the distillation method is mainly used, but the online regeneration is not feasible, and the regeneration needs to be replaced for separate disposal, thus the labor and the time are wasted. The common practice for regenerating waste activated carbon is to use steam heating for activating regeneration or high-temperature roasting, and the aim of activating regeneration can be achieved for high-temperature roasting, oxidizing and separating and desorbing organic matters because the organic matters used for extraction are all high-boiling matters and cannot be achieved by steam heating, but the investment and operation cost is relatively high, and the aim of recovering lost organic phases is not achieved.
Aiming at the defects of the prior art and the process, and particularly aiming at the higher requirements on quality, safety, environmental protection and industrial automation in the current economic form, the invention provides an on-line recovery process and device for the lost organic phase of a hydrometallurgical extraction separation system. Firstly, ultrasonic oscillation is adopted to break emulsion, and then a super oleophobic hydrophilic membrane is adoptedMore than 95% of oil drops can be separated on line, residual oil drops and dissolved organic matters are adsorbed by the combination of adsorption fiber balls and activated carbon, and only one of the oil drops can be used according to working conditions. The adsorption process adopts A, B line combination without stopping production, utilizes supercritical carbon dioxide extraction technology to recover the lost organic matters adsorbed on the fiber balls and the activated carbon on line, and achieves the aim of activating and adsorbing the fiber balls and the activated carbon on line so as to repeatedly use the fiber balls and the activated carbon. Organic matters such as extractant and solvent coal oil can be eluted from the adsorption fiber balls and the activated carbon at room temperature by adopting a supercritical carbon dioxide extraction technology, the organic matters can not be destroyed, the supercritical carbon dioxide can be returned to a system for reuse, the aim of regenerating the adsorption fiber balls and the activated carbon can be completely achieved due to the super-strong solubility and penetrability of the supercritical carbon dioxide, and even the regenerated fiber balls and the activated carbon have stronger adsorption capacity. The product treated by the process has better quality, the oil content of the treated product solution is less than 0.5ppm, the COD is less than 30mg/L, the COD in the wastewater can be reduced to below 30mg/L, and the VOCs in the waste gas can be reduced to 50 mg/m 3 The following is given. Because the whole process of the process is to operate liquid phase or gas phase fluid, automation is easy to realize, and a foundation is laid for on-line recovery and loss of organic phase.
The invention adopts supercritical carbon dioxide extraction technology to recycle the lost organic phase on line in the hydrometallurgical extraction separation system, and the whole process can realize automatic production control, thereby not only improving the production efficiency, but also recycling the lost raw materials, reducing the production cost, improving the product quality, and simultaneously reducing the COD of the waste water and the VOCs in the waste gas to the level of environmental protection requirement.
It should be noted that carbon dioxide is in a non-gaseous and non-liquid state at a temperature higher than 31.1 ℃ and a pressure higher than 7.39MPa, which is a supercritical state, and carbon dioxide is a supercritical carbon dioxide fluid.
All components and equipment of the present invention, unless otherwise specified, are all components and equipment known in the art, such as hydrometallurgical extraction separation systems known in the art. The organic phase in the invention is common organic phase in hydrometallurgical extraction separation systems. Valves are arranged on the pipelines.
The following specific embodiments of the present invention are provided, and it should be noted that the present invention is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical solutions of the present application fall within the protection scope of the present invention.
Example 1:
the embodiment provides an on-line recovery device for a lost organic phase of a hydrometallurgical extraction separation system, which comprises a product water phase or wastewater phase lost organic phase recovery sub-device 1 and an acid mist waste gas lost organic phase recovery sub-device 2.
As shown in fig. 1, the product water phase or wastewater phase lost organic phase recovery sub-device 1 comprises a temporary storage tank 101 connected with a pipeline 3 of a product water phase or wastewater phase in a hydrometallurgical extraction separation system, wherein the temporary storage tank 101 is connected with a liquid inlet of an ultrasonic demulsifier 103 through a water pump 102, a liquid outlet of the ultrasonic demulsifier 103 is connected with a feed inlet of a super-oleophobic hydrophilic membrane separator 104, an organic phase outlet at the upper end of the super-oleophobic hydrophilic membrane separator 104 is connected with an organic phase collecting tank 105, a water phase outlet at the lower end of the super-oleophobic hydrophilic membrane separator 104 is connected with a bottom valve of a fiber ball adsorption tower 106, a discharge outlet at the upper end of the fiber ball adsorption tower 106 is connected with a bottom valve of a first activated carbon adsorption tower 107, and a discharge outlet at the upper end of the first activated carbon adsorption tower 107 is connected with a pipeline 4 of a next process in the hydrometallurgical extraction separation system;
the inlets at the upper ends of the fiber ball adsorption tower 106 and the first activated carbon adsorption tower 107 are respectively connected with a first liquid carbon dioxide pipeline 109 with a first flowmeter 108; the bottom valve of the fiber ball adsorption tower 106 is connected with the first organic matter recovery tank 110, and the bottom valve of the first activated carbon adsorption tower 107 is connected with the second organic matter recovery tank 111;
as shown in fig. 2, the organic phase recovery sub-device 2 for the loss of acid mist waste gas comprises a second active carbon adsorption tower 201, wherein a bottom valve of the second active carbon adsorption tower 201 is used for being connected with a pipeline 5 of acid mist waste gas in an induced air system in a hydrometallurgical extraction separation system, and a discharge port at the upper end of the second active carbon adsorption tower 201 is connected with a pipeline 6 of an acid mist absorption process in the hydrometallurgical extraction separation system;
the upper inlet of the second activated carbon adsorption tower 201 is connected with a second liquid carbon dioxide pipeline 203 with a second flowmeter 202; the bottom valve of the second activated carbon adsorption column 201 is connected to a third organic recovery tank 204.
As a preferable aspect of the present embodiment, a return pipe 112 is further provided between the ultrasonic demulsifier 103 and the temporary storage tank 101.
As a preferable aspect of the present embodiment, the inlets at the upper ends of the fiber ball adsorption tower 106 and the first activated carbon adsorption tower 107 are also respectively communicated with the first gaseous carbon dioxide pipeline 113. The upper inlet of the second activated carbon adsorption column 201 is also connected to a second gaseous carbon dioxide conduit 205. Before the supercritical carbon dioxide extraction and regeneration process, gaseous carbon dioxide is adopted to discharge water phase or waste water phase of the product, and residual water in relevant equipment in the organic phase recovery sub-device 1 and the acid mist waste gas is lost.
As a preferable scheme of the present embodiment, the fiber ball adsorption tower 106, the first activated carbon adsorption tower 107 and the second activated carbon adsorption tower 201 are all arranged in parallel one by one.
As a preferable mode of the present embodiment, the fiber ball adsorption tower 106, the first activated carbon adsorption tower 107, the second activated carbon adsorption tower 201, the first organic matter recovery tank 110, the second organic matter recovery tank 111, and the third organic matter recovery tank 204 are each provided with a temperature control jacket, a thermometer, a pressure gauge, a safety valve, and/or a purge valve, and a heating belt is provided after the purge valve.
Example 2:
the embodiment provides an on-line recovery process of an organic phase lost by a hydrometallurgical extraction separation system, which comprises a recovery process of the organic phase lost in a product water phase, a recovery process of the organic phase lost in a wastewater phase and a recovery process of the organic phase lost in acid mist waste gas;
the recovery process of the lost organic phase in the product water phase is the same as that of the lost organic phase in the wastewater phase, and the product water phase or the lost organic phase recovery sub-device 1 in the wastewater phase is adopted;
after entering a temporary storage tank 101, a product water phase or wastewater phase is sent into an ultrasonic demulsifier 103 through a water pump 102 to be demulsified, then enters a super oleophobic hydrophilic membrane separator 104 to be separated from an organic phase, the organic phase enters an organic phase collecting tank 105, the water phase enters a fiber ball adsorption tower 106 and a first activated carbon adsorption tower 107 to adsorb organic matters in the water phase, and the water phase after passing through the first activated carbon adsorption tower 107 enters the next procedure in a hydrometallurgical extraction separation system;
when regeneration is needed after adsorption is completed, gaseous carbon dioxide is firstly adopted to discharge water phase or waste water phase of the product, and residual water in relevant equipment in the organic phase loss recovery sub-device 1 is recovered. Then, introducing liquid carbon dioxide into the fiber ball adsorption tower 106 and the first activated carbon adsorption tower 107, regulating the liquid carbon dioxide into a supercritical state in the fiber ball adsorption tower 106 and the first activated carbon adsorption tower 107, and extracting organic matters adsorbed in the fiber ball adsorption tower 106 and the first activated carbon adsorption tower 107 by using carbon dioxide supercritical to regenerate the fiber balls in the fiber ball adsorption tower 106 and the activated carbon in the first activated carbon adsorption tower 107, wherein the extracted organic matters enter a first organic matter recovery tank 110 and a second organic matter recovery tank 111;
the recovery process of the lost organic phase in the acid mist waste gas adopts the recovery sub-device 2 of the lost organic phase in the acid mist waste gas, which is given in the embodiment 1;
the acid mist waste gas enters a second activated carbon adsorption tower 201 to adsorb organic matters in the acid mist waste gas, and the acid mist waste gas after passing through the second activated carbon adsorption tower 201 enters an acid mist absorption process in a hydrometallurgical extraction separation system;
when regeneration is needed after adsorption is completed, gaseous carbon dioxide is firstly adopted to discharge water and air remained in relevant equipment in the organic phase recovery sub-device 2 which is used for losing the acid mist waste gas. Liquid carbon dioxide is introduced into the second activated carbon adsorption tower 201, the liquid carbon dioxide is regulated to a supercritical state in the second activated carbon adsorption tower 201, and organic matters adsorbed in the second activated carbon adsorption tower 201 are extracted by carbon dioxide supercritical, so that activated carbon in the second activated carbon adsorption tower 201 is regenerated, and the organic matters obtained by extraction enter a third organic matter recovery tank 204.
As a preferred scheme of this embodiment, the ultrasonic demulsification process conditions in the ultrasonic demulsifier 103 are as follows: the ultrasonic frequency is 20-25 KHz, the residence time of the product water phase or waste water phase in the ultrasonic demulsifier 103 is less than 15min, and the flow rate of the product water phase or waste water phase and the position of the overflow port of the product water phase or waste water phase are controlled.
As a preferred embodiment of the present embodiment, the pore size of the super oleophobic hydrophilic membrane in the super oleophobic hydrophilic membrane separator 104 is 0.5-15 microns.
As a preferable scheme of this embodiment, the process conditions of the supercritical carbon dioxide extraction regeneration are: the pressure is 7.39-15.9 Mpa, the temperature is 31.1-65 ℃, and the supercritical carbon dioxide extraction residence time is 15-180 min.
Example 3:
the embodiment provides an on-line recovery process of the lost organic phase of the hydrometallurgical extraction separation system based on the embodiment 2, wherein the process comprises an on-line recovery process of the lost organic phase of the product aqueous phase, and the product aqueous phase in the embodiment is a cobalt sulfate aqueous solution, namely the embodiment provides an on-line recovery process of the lost organic phase of the cobalt sulfate aqueous solution in the hydrometallurgical extraction separation system.
In this example, the aqueous cobalt sulfate solution from the extraction line contained extractant P507 and solvent kerosene, and was recovered on-line using the process of example 2. Wherein, the fibrous ball adsorption tower 106 and the active carbon adsorption tower 107 are provided one by one, organic matters contained in the cobalt sulfate aqueous solution after flowing out according to the flow are separated and adsorbed in a segmented way, the organic matters contained in the cobalt sulfate aqueous phase at the outlet are less than or equal to 0.5ppm, and the COD is less than or equal to 30mg/L.
Example 4:
the embodiment provides an on-line recovery process of the lost organic phase of the hydrometallurgical extraction separation system based on the embodiment 2, wherein the process comprises a recovery process of the lost organic phase of the wastewater phase, and the wastewater phase in the embodiment is raffinate, namely the embodiment provides an on-line recovery process of the raffinate lost organic phase in the hydrometallurgical extraction separation system.
In this example, the raffinate was adjusted to ph=3.5 prior to treatment.
On-line recovery was carried out in the same manner as in example 3, with a COD of the aqueous phase at the outlet after treatment of less than or equal to 30mg/L.
Example 5:
the embodiment provides an on-line recovery process of the lost organic phase based on the hydrometallurgical extraction separation system of the embodiment 2, wherein the process comprises the recovery process of the lost organic phase in acid mist waste gas.
The process of example 2 was used for on-line recovery. The outlet VOCs of the acid mist waste gas in the extraction section after the acid mist waste gas is adsorbed by the activated carbon is less than or equal to 25mg/m 3 。
Example 6:
this example shows an on-line recovery process of the lost organic phase based on the hydrometallurgical extraction separation system of example 2, which includes on-line regeneration of the fiber balls in the fiber ball adsorption column 106.
When the adsorption of the fiber balls is saturated (whether the fiber balls are saturated or not can be known by detecting the COD of the solution before and after the fiber ball adsorption tower), the adsorbed organic matters are required to be regenerated and recovered on line.
The corresponding valve was closed and opened, and the aqueous phase remaining in the fiber ball adsorption column 106 was slowly pressed out by gaseous carbon dioxide and the pressure was raised to 0.8Mpa. Then, liquid carbon dioxide is introduced to 8Mpa, the temperature of the system is kept at 35 ℃, at the moment, the carbon dioxide in the system is in a supercritical state, the density is 0.4, the state is kept for 1h, then the system is cooled to 20 ℃, at the moment, the carbon dioxide is in a liquid state, the density is 0.8, because the volume of the first organic matter recovery tank 110 is larger than that of the adsorption tower, the carbon dioxide which extracts organic matters falls into the first organic matter recovery tank 110 in a liquid state, a cut-off valve between the fiber ball adsorption tower 106 and the first organic matter recovery tank 110 is closed, the temperature is kept at 20-25 ℃, the carbon dioxide is discharged through a vent valve of the first organic matter recovery tank 110 (at the same time, the heating belt is opened to ensure that the carbon dioxide does not freeze in the releasing process), the extracted organic matters remain in the first organic matter recovery tank 110, and the extracted organic matters are discharged through a bottom valve and returned to the system.
Then closing the emptying valve and the bottom valve, opening the cutting valve between the fiber ball adsorption tower 106 and the first organic matter recovery tank 110, continuing to feed liquid carbon dioxide into the fiber ball adsorption tower 106 to 8Mpa, keeping the temperature of the system at 35 ℃, keeping the supercritical state of the carbon dioxide in the system for 1h, cooling the system to 20 ℃, allowing the carbon dioxide with the organic matters extracted for the second time to fall into the first organic matter recovery tank 110 in the liquid state, closing the cutting valve between the fiber ball adsorption tower 106 and the first organic matter recovery tank 110, keeping the temperature at 20-25 ℃, discharging the carbon dioxide through the emptying valve of the first organic matter recovery tank 110, and discharging the extracted organic matters in the first organic matter recovery tank 110 and returning the extracted organic matters to the system through the bottom valve. And opening the emptying valve to discharge residual carbon dioxide in the fiber ball adsorption tower 106, and completing the fiber ball regeneration process for standby.
The regenerated fiber balls contain 0.35 percent of organic matters, the untreated adsorption saturated fiber balls contain 9.5 percent of organic matters, and the deoiling rate is 96.3 percent.
Examples 7 to 9:
this example shows an on-line recovery process of the lost organic phase based on the hydrometallurgical extraction separation system of example 2, which includes on-line regeneration of the fiber balls in the fiber ball adsorption column 106.
The process of this example is essentially the same as that of example 6, except that the specific process conditions are different, as shown in Table 1 below.
Examples 10 to 15:
this example shows an on-line recovery process of the lost organic phase based on the hydrometallurgical extraction separation system of example 2, which includes on-line regeneration of the activated carbon in the first activated carbon adsorption column 107.
When the activated carbon is saturated (whether the activated carbon is saturated or not can be known by detecting COD of the solution before and after the activated carbon adsorption tower or whether the activated carbon is saturated or not can be known by detecting VOCs in the acid mist before and after the activated carbon adsorption tower) the organic matters adsorbed by the activated carbon are regenerated and recovered on line.
The process of this example was substantially the same as that of example 6, except that the regenerated object in this example was activated carbon, and specific process conditions were different, as shown in table 2 below.
Note that: adsorption capacity = extractant/activated carbon x 100%.
Claims (9)
1. The process is characterized by comprising a product water phase lost organic phase recovery process, a wastewater phase lost organic phase recovery process and an acid mist waste gas lost organic phase recovery process;
the recovery process of the lost organic phase in the product water phase is the same as that of the lost organic phase in the wastewater phase, and a product water phase or wastewater phase lost organic phase recovery sub-device (1) is adopted;
the product water phase or wastewater phase loss organic phase recovery sub-device (1) comprises a temporary storage tank (101) which is connected with a pipeline (3) of a product water phase or wastewater phase in a hydrometallurgical extraction separation system, the temporary storage tank (101) is connected with a liquid inlet of an ultrasonic demulsifier (103) through a water pump (102), a liquid outlet of the ultrasonic demulsifier (103) is connected with a feed inlet of a super-oleophobic hydrophilic membrane separator (104), an organic phase outlet at the upper end of the super-oleophobic hydrophilic membrane separator (104) is connected with an organic phase collecting tank (105), a water phase outlet at the lower end of the super-oleophobic hydrophilic membrane separator (104) is connected with a bottom valve of a fiber ball adsorption tower (106), a discharge outlet at the upper end of the fiber ball adsorption tower (106) is connected with a bottom valve of a first activated carbon adsorption tower (107), and a discharge outlet at the upper end of the first activated carbon adsorption tower (107) is connected with a pipeline (4) of a next process in the hydrometallurgical extraction separation system;
the upper end inlets of the fiber ball adsorption tower (106) and the first activated carbon adsorption tower (107) are respectively connected with a first liquid carbon dioxide pipeline (109) with a first flowmeter (108); the bottom valve of the fiber ball adsorption tower (106) is connected with a first organic matter recovery tank (110), and the bottom valve of the first activated carbon adsorption tower (107) is connected with a second organic matter recovery tank (111);
after entering a temporary storage tank (101), a product water phase or a wastewater phase is sent into an ultrasonic demulsifier (103) through a water pump (102) to be demulsified, then enters a super oleophobic hydrophilic membrane separator (104) to be separated from an organic phase and a water phase, the organic phase enters an organic phase collecting tank (105), the water phase enters a fiber ball adsorption tower (106) and a first activated carbon adsorption tower (107) to adsorb organic matters in the water phase, and the water phase after passing through the first activated carbon adsorption tower (107) enters the next working procedure in a hydrometallurgical extraction separation system;
when regeneration is needed after adsorption is completed, introducing liquid carbon dioxide into the fiber ball adsorption tower (106) and the first activated carbon adsorption tower (107), regulating the liquid carbon dioxide into a supercritical state in the fiber ball adsorption tower (106) and the first activated carbon adsorption tower (107), and extracting organic matters adsorbed in the fiber ball adsorption tower (106) and the first activated carbon adsorption tower (107) by using carbon dioxide supercritical to regenerate the fiber balls in the fiber ball adsorption tower (106) and the activated carbon in the first activated carbon adsorption tower (107), wherein the organic matters obtained by extraction enter a first organic matter recovery tank (110) and a second organic matter recovery tank (111);
the recovery process of the lost organic phase in the acid mist waste gas adopts an organic phase recovery sub-device (2) for lost organic phase in the acid mist waste gas;
the organic phase recovery sub-device (2) for the loss of the acid mist waste gas comprises a second active carbon adsorption tower (201), wherein a bottom valve of the second active carbon adsorption tower (201) is used for being connected with a pipeline (5) of the acid mist waste gas in an induced air system in a hydrometallurgical extraction separation system, and a discharge port at the upper end of the second active carbon adsorption tower (201) is connected with a pipeline (6) of an acid mist absorption procedure in the hydrometallurgical extraction separation system;
the upper end inlet of the second activated carbon adsorption tower (201) is connected with a second liquid carbon dioxide pipeline (203) with a second flowmeter (202); the bottom valve of the second activated carbon adsorption tower (201) is connected with a third organic matter recovery tank (204);
the acid mist waste gas enters a second activated carbon adsorption tower (201) to adsorb organic matters in the acid mist waste gas, and the acid mist waste gas after passing through the second activated carbon adsorption tower (201) enters an acid mist absorption procedure in a hydrometallurgical extraction separation system;
when regeneration is needed after adsorption is completed, liquid carbon dioxide is introduced into the second activated carbon adsorption tower (201), the liquid carbon dioxide is regulated to a supercritical state in the second activated carbon adsorption tower (201), and organic matters adsorbed in the second activated carbon adsorption tower (201) are extracted by carbon dioxide supercritical, so that activated carbon in the second activated carbon adsorption tower (201) is regenerated, and the organic matters obtained by extraction enter a third organic matter recovery tank (204).
2. The on-line recovery process of lost organic phase of hydrometallurgical extraction separation system according to claim 1, wherein the ultrasonic demulsification process conditions in the ultrasonic demulsifier (103) are as follows: the ultrasonic frequency is 20-25 KHz, the residence time of the product water phase or waste water phase in the ultrasonic demulsifier (103) is less than 15min, and the flow rate of the product water phase or waste water phase and the position of the overflow port of the product water phase or waste water phase are controlled.
3. The hydrometallurgical extraction separation system lost organic phase online recovery process according to claim 1, wherein the aperture of the super oleophobic hydrophilic membrane in the super oleophobic hydrophilic membrane separator (104) is 0.5-15 microns.
4. The hydrometallurgical extraction separation system lost organic phase online recovery process according to claim 1, wherein the process conditions of supercritical carbon dioxide extraction are as follows: the pressure is 7.39-15.9 Mpa, the temperature is 31.1-65 ℃, and the supercritical carbon dioxide extraction residence time is 15-180 min.
5. The on-line recovery process of lost organic phase of hydrometallurgical extraction separation system according to claim 1, wherein a return pipe (112) is further arranged between the ultrasonic demulsifier (103) and the temporary storage tank (101).
6. The on-line recovery process of lost organic phase of hydrometallurgical extraction separation system according to claim 1, wherein the inlets at the upper ends of the fiber ball adsorption tower (106) and the first activated carbon adsorption tower (107) are also respectively communicated with a first gaseous carbon dioxide pipeline (113).
7. The hydrometallurgical extraction separation system lost organic phase on-line recovery process according to claim 1, wherein the upper inlet of the second activated carbon adsorption tower (201) is further connected to a second gaseous carbon dioxide conduit (205).
8. The hydrometallurgical extraction separation system lost organic phase online recovery process according to claim 1, wherein the fiber ball adsorption tower (106), the first activated carbon adsorption tower (107) and the second activated carbon adsorption tower (201) are all arranged in parallel.
9. The hydrometallurgical extraction separation system loss organic phase online recovery process according to claim 1, wherein the fiber ball adsorption tower (106), the first activated carbon adsorption tower (107), the second activated carbon adsorption tower (201), the first organic matter recovery tank (110), the second organic matter recovery tank (111) and the third organic matter recovery tank (204) are respectively provided with a temperature control jacket, a thermometer, a pressure gauge, a safety valve and/or a blow valve, and a heating belt is arranged behind the blow valve.
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