CN109022794B - Process and device for recovering precious metals in waste catalyst - Google Patents
Process and device for recovering precious metals in waste catalyst Download PDFInfo
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- CN109022794B CN109022794B CN201810656335.7A CN201810656335A CN109022794B CN 109022794 B CN109022794 B CN 109022794B CN 201810656335 A CN201810656335 A CN 201810656335A CN 109022794 B CN109022794 B CN 109022794B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
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Abstract
The invention provides a recovery process and a recovery device of precious metals in a waste catalyst, wherein the recovery process of the precious metals in the waste catalyst is to directly oxidize and separate a liquid-phase waste catalyst in a strong acid environment by utilizing hydrogen peroxide so as to recover the precious metal rhodium; a recovery device for precious metals in waste catalysts comprises a reaction kettle, a waste catalyst solution inlet pipeline, a hydrogen peroxide inlet pipeline, a sulfuric acid inlet pipeline, a reaction kettle top outlet pipeline, a reaction kettle bottom outlet pipeline, a reaction kettle jacket, a phase separator, an incineration system, a concentration system, a catalyst manufacturing process, an elevated tank, a condenser, a water seal tank, an odor recovery system, a steam inlet pipeline, a steam outlet pipeline and a desalted water inlet pipeline; the operation is simple, the reaction is complete, the total time consumption of the whole process is 5-10h, and the recovery rate reaches 95-98%.
Description
Technical Field
The invention relates to the field of precious metal recovery, in particular to a process and a device for recovering precious metal rhodium in a waste catalyst.
Technical Field
Rhodium-containing catalysts are widely applied to the carbonylation of methanol to prepare acetic acid and the hydroformylation of olefins, and because rhodium metal is a rare metal with high price, the catalysts can be continuously aged in the using process, if noble metal rhodium in the aged catalysts is not recycled, the loss of the noble metal rhodium is caused, and therefore, the problem of recycling the noble metal rhodium in the aged catalysts needs to be solved. Patent CN148522 describes a method for recovering noble metals from waste catalysts, which comprises leaching pretreated catalysts with a mixture of hydrogen peroxide, hydrogen ions and chloride ion solutions to make noble metal components exist in the mixed solution in an ionic state, and finally treating the noble metal solution to recover noble metals. The method mainly aims at the Pt and Pd catalysts, only one step of leaching is carried out for 12 hours, the catalysts need to be processed from a liquid state to a solid simple substance state, roasting is mostly needed when the catalysts are processed to the solid state, and the processing process is complex and laborious.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a process for recovering noble metal rhodium in a waste catalyst, which utilizes hydrogen peroxide to directly oxidize and separate a liquid-phase waste catalyst in a strong acid environment so as to recover the noble metal rhodium.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a recovery process of noble metal rhodium in a waste catalyst, which comprises the following specific steps:
(1) oxidation preliminary separation stage: pumping a certain volume of waste catalyst solution into a reaction kettle by a pump, adding 98% sulfuric acid into the reaction kettle while stirring, slowly heating to 30-40 ℃, then adding hydrogen peroxide into the reaction kettle, preserving heat for 2-3 hours, fully separating noble metal rhodium from a ligand thereof, allowing the noble metal rhodium to enter a water phase and the ligand to enter an oil phase, and cooling gas generated by reaction and then sending the cooled gas to a peculiar smell recovery system for treatment.
Further, the volume of the 98 percent sulfuric acid is 10 to 20 percent of the volume of the waste catalyst solution.
Furthermore, the adding speed of the 98% sulfuric acid is controlled to be 1-1.5L/s.
Furthermore, the stirring speed is controlled to be 60-80 r/min.
Furthermore, the volume of hydrogen peroxide is 30-50% of the volume of the waste catalyst solution respectively.
Furthermore, the concentration of the hydrogen peroxide is 25 to 30 weight percent.
Furthermore, the adding speed of the hydrogen peroxide is controlled to be 0.8-1.2L/s.
Furthermore, the stirring speed is controlled to be 60-80 r/min.
Further, the temperature of the reaction kettle is 90-120 ℃.
Furthermore, the temperature of the reaction kettle is controlled by adjusting the steam input amount of the jacket of the reaction kettle.
Furthermore, the reaction kettle is provided with an overtemperature interlocking system, the interlocking value is 120 ℃, if the interlocking value is higher than the interlocking value, hydrogen peroxide and steam feeding valves are closed, a desalted water feeding pipeline is opened, and the system is cooled, so that the safety and the reliability of the oxidation reaction are ensured.
Further, the pressure of the reaction kettle is 0-0.1 MPa.
Furthermore, the reaction kettle is provided with an overpressure interlocking system, the interlocking value is 0.1MPa, if the interlocking value is higher than the interlocking value, hydrogen peroxide and steam feeding valves are closed, a desalted water feeding pipeline is opened, the temperature and the pressure of the system are reduced, and the safety and the reliability of the oxidation reaction are ensured.
Further, gas generated by reaction is buffered by the elevated tank and then enters the condenser for cooling, condensed liquid enters a water seal, and a small amount of non-condensable gas enters the peculiar smell recovery system.
Furthermore, an oxygen online monitoring system is arranged, when the oxygen concentration reaches 5%, hydrogen peroxide and steam feeding valves are closed, a desalted water feeding pipeline is opened, and the system is cooled to ensure the safety and reliability of the oxidation reaction.
(2) Oxidation enhanced separation stage: adding hydrogen peroxide at the speed of 0.8-1.2L/s to continue the reaction, and keeping the temperature for 2-3 h.
Furthermore, the volume of the added hydrogen peroxide is 40-60% of the volume of the waste catalyst solution.
Further, the concentration of hydrogen peroxide is 25-30 wt.%.
Furthermore, the stirring speed is controlled to be 60-80 r/min.
(3) A sampling analysis stage: sampling to detect the rhodium content in the oil phase, and if the rhodium content is less than 5ppm, pumping the waste catalyst solution into a phase separator to stand for 30-50min for extraction and separation; and (3) if the rhodium content in the oil phase is more than 5ppm, adding hydrogen peroxide, and repeating the step (2) to completely react until the rhodium content is qualified.
(4) A concentration and recovery stage: and after extraction, sending the oil phase to a burning system, sending the water phase to a concentration system for concentration to remove excessive water, and then sending to a catalyst preparation process to prepare a new catalyst.
The invention also provides a device for realizing the process, which comprises a reaction kettle, a phase separator and a head tank, wherein the side wall of the reaction kettle is sequentially provided with inlets for sulfuric acid, hydrogen peroxide and waste catalyst solution from top to bottom, the inlets for the sulfuric acid, the hydrogen peroxide and the waste catalyst solution of the reaction kettle are sequentially connected with pipelines for the sulfuric acid, the hydrogen peroxide and the waste catalyst solution, the gas phase outlet at the top of the reaction kettle is sequentially connected with the head tank, a condenser and a water seal tank, the gas phase outlet at the top of the reaction kettle is connected with the inlet of the head tank, the outlet of the head tank is connected with the inlet of the condenser, the outlet of the condenser is connected with the water seal tank, the outlet of the water seal tank is connected with an odor recovery system, the liquid phase outlet at the bottom of the reaction kettle is connected with the inlet of the phase separator, the oil phase outlet of the phase separator, the outlet of the concentration system is connected with the inlet of the catalyst manufacturing procedure.
The invention has the beneficial effects that:
1. the method has the advantages of simple operation, full reaction, total time consumption of 5-10h in the whole process, and recovery rate of 95-98%.
2. The invention is provided with the safety interlocking control system, realizes automatic control and improves the intrinsic safety level of the device.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
Fig. 1 is a schematic structural view of a recovery apparatus for precious metals from the spent catalyst.
The system comprises a reaction kettle 1, a reaction kettle 2, a waste catalyst solution inlet pipeline 3, a hydrogen peroxide inlet pipeline 4, a sulfuric acid inlet pipeline 5, a reaction kettle top outlet pipeline 6, a reaction kettle bottom outlet pipeline 7, a reaction kettle jacket 8, a phase separator 9, an incineration system 10, a concentration system 11, a catalyst manufacturing process 12, an elevated tank 13, a condenser 14, a water seal tank 15, an odor recovery system 16, a steam inlet pipeline 17, a steam outlet pipeline 18 and a desalted water inlet pipeline.
The specific process is shown in the following examples.
Example 1:
the 20L of waste catalyst-containing solution generated in the process of preparing acetic acid by methanol carbonylation is firstly pumped into a reaction kettle 1 by a pump through a waste catalyst solution inlet pipeline 2, then 98 percent sulfuric acid 3L is added into the reaction kettle 1 from a sulfuric acid inlet pipeline 4 at the speed of 1.2L/s while stirring, a steam inlet pipeline 16 is opened, steam is introduced into a reaction kettle jacket, the temperature is slowly increased to 32 ℃, then 20L of 27.5 wt.% hydrogen peroxide is added into the reaction kettle 1 from a hydrogen peroxide inlet pipeline 3 at the speed of 0.9L/s, and the temperature of the reaction kettle is stabilized at 100 ℃ by controlling the introduction amount of the steam in the reaction kettle jacket 7.
After the heat preservation is carried out for 2.3 hours, 8.5 L27.5wt.% of hydrogen peroxide is added into the reaction kettle 1 from the hydrogen peroxide inlet pipeline 3 at the speed of 0.9L/s to continue the reaction, the heat preservation is carried out for 2.5 hours, the sampling detection shows that the rhodium content in the oil phase is 4ppm, the sample is qualified, the treated waste catalyst solution is pumped into a phase separator 8 from an outlet pipeline 6 at the bottom of the reaction kettle for extraction and separation, the extraction time is 40min, the oil phase is sent to an incineration system 9 after the extraction is finished, the water phase is sent to a concentration system 10 for concentration to remove the redundant moisture, and then the waste catalyst solution is sent to a catalyst preparation process 11 to prepare a new catalyst.
Gas generated in the reaction process is buffered by an overhead tank 12 through an outlet pipeline 5 at the top of the reaction kettle, enters a condenser 13, is condensed, enters a water seal tank 14, and a small amount of residual gas enters an odor recovery system 15.
The recovery of noble metal rhodium was calculated to be 96%.
Example 2:
50L of waste catalyst-containing solution generated in the olefin hydroformylation reaction process is firstly pumped into a reaction kettle 1 through a waste catalyst solution inlet pipeline 2 by a pump, then 8L of 98 percent sulfuric acid is added into the reaction kettle 1 from a sulfuric acid inlet pipeline 4 at the speed of 1.3L/s while stirring, a steam inlet pipeline 16 is opened, steam is introduced into a reaction kettle jacket, the temperature is slowly increased to 35 ℃, then 20L of 29.5 wt.% hydrogen peroxide is added into the reaction kettle 1 from a hydrogen peroxide inlet pipeline 3 at the speed of 1.0L/s, and the temperature of the reaction kettle is stabilized at 110 ℃ by controlling the introduction amount of the steam in the reaction kettle jacket 7.
After the heat preservation is carried out for 2.5 hours, 25 L29.5wt.% of hydrogen peroxide is added into the reaction kettle 1 from the hydrogen peroxide inlet pipeline 3 at the speed of 1L/s to continue the reaction, the heat preservation is carried out for 2.6 hours, the sampling is carried out to detect that the content of rhodium in the oil phase is 3ppm, the sample is qualified, the treated waste catalyst solution is pumped into a phase separator 8 from an outlet pipeline 6 at the bottom of the reaction kettle to carry out extraction and separation, the extraction time is 50min, the oil phase is sent to an incineration system 9 after the extraction is finished, the water phase is sent to a concentration system 10 to carry out concentration to remove excess moisture, and then the waste catalyst solution is sent to a catalyst preparation process 11 to.
Gas generated in the reaction process is buffered by an overhead tank 12 through an outlet pipeline 5 at the top of the reaction kettle, enters a condenser 13, is condensed, enters a water seal tank 14, and a small amount of residual gas enters an odor recovery system 15.
The recovery of noble metal rhodium was calculated to be 98%.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (3)
1. A recovery process of precious metal in waste catalyst is characterized in that hydrogen peroxide is used to directly oxidize and separate liquid phase waste catalyst in strong acid environment, thereby recovering precious metal rhodium, and the specific process steps are as follows:
(1) oxidation preliminary separation stage: pumping a certain volume of waste catalyst solution into a reaction kettle by a pump, adding 98% sulfuric acid into the reaction kettle while stirring, slowly heating to 30-40 ℃, then adding hydrogen peroxide into the reaction kettle, preserving heat for 2-3 hours, fully separating noble metal rhodium from a ligand thereof, allowing the noble metal rhodium to enter a water phase and the ligand to enter an oil phase, cooling gas generated by reaction, and then sending the cooled gas to a peculiar smell recovery system for treatment; the volume of the 98 percent sulfuric acid is 10 to 20 percent of the volume of the waste catalyst solution, the adding speed of the 98 percent sulfuric acid is controlled to be 1 to 1.5L/s, and the stirring speed is controlled to be 60 to 80 r/min; the volume of hydrogen peroxide is 30-50% of the volume of the waste catalyst solution, the concentration of hydrogen peroxide is 25-30 wt%, the adding speed of hydrogen peroxide is controlled to be 0.8-1.2L/s, and the stirring speed is controlled to be 60-80 r/min; the temperature of the reaction kettle is 90-120 ℃, and the pressure of the reaction kettle is 0-0.1 MPa;
(2) oxidation enhanced separation stage: adding hydrogen peroxide at the speed of 0.8-1.2L/s to continue the reaction, and keeping the temperature for 2-3 h;
(3) a sampling analysis stage: sampling to detect the rhodium content in the oil phase, and if the rhodium content is less than 5ppm, pumping the waste catalyst solution into a phase separator to stand for 30-50min for extraction and separation; if the rhodium content in the oil phase is more than 5ppm, adding hydrogen peroxide to repeat the step (2) to ensure that the reaction is complete until the rhodium content is qualified;
(4) a concentration and recovery stage: after extraction, sending the oil phase to a burning system, sending the water phase to a concentration system for concentration to remove excessive water, and then sending to a catalyst manufacturing procedure to manufacture a new catalyst;
the process steps from step (1) to step (4) are realized by adopting the following recovery device: including reation kettle, phase separator, elevated tank, reation kettle lateral wall from the top down sets gradually sulphuric acid, hydrogen peroxide solution, useless catalyst solution import, reation kettle's sulphuric acid, hydrogen peroxide solution, useless catalyst solution import connect gradually sulphuric acid, hydrogen peroxide solution, useless catalyst solution pipeline, the elevated tank is connected gradually to the gaseous phase export at reation kettle top, the condenser, the water seal pond, the gaseous phase export at reation kettle top and the access connection of elevated tank, the export of elevated tank and the access connection of condenser, the condenser export is connected with the water seal pond, the water seal pond export is connected with peculiar smell recovery system, the liquid phase export and the phase separator access connection of reation kettle bottom, the oil phase export and the system access connection that burns of phase separator, the water phase export and the concentrated system access connection of phase separator, concentrated system export and catalyst preparation process access connection.
2. The process for recovering the noble metals in the waste catalyst according to claim 1, wherein the reaction kettle in the step (1) is provided with an overtemperature interlocking system, the interlocking value is 120 ℃, if the interlocking value is higher than the interlocking value, hydrogen peroxide and steam feeding valves are closed, and a desalted water feeding pipeline is opened; the reaction kettle is provided with an overpressure interlocking system, the interlocking value is 0.1MPa, if the interlocking value is higher than the interlocking value, hydrogen peroxide and steam feeding valves are closed, and a desalted water feeding pipeline is opened.
3. The process for recovering the noble metals in the waste catalyst according to claim 1, wherein an oxygen on-line monitoring system is arranged in the reaction kettle in the step (1), and when the oxygen concentration reaches 5%, hydrogen peroxide and steam feeding valves are closed, and a desalted water feeding pipeline is opened.
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| CN105944768A (en) * | 2016-05-10 | 2016-09-21 | 能特科技有限公司 | Method for recovering rhodium catalyst from rhodium-containing wastewater |
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| CN1072729C (en) * | 1996-12-13 | 2001-10-10 | 抚顺石油化工公司洗涤剂化工厂 | Method for recovering cobalt from cobalt contg. waste catalyst used is carbonylation syntehsizing process |
| CN102277499B (en) * | 2011-08-11 | 2012-12-26 | 杭州凯大催化金属材料有限公司 | Method for recovering rhodium from organic waste liquid produced in carbonyl synthesis reaction |
| JP6780448B2 (en) * | 2016-11-02 | 2020-11-04 | 住友金属鉱山株式会社 | How to recover high-grade rhodium powder |
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| CN1448522A (en) * | 2002-04-04 | 2003-10-15 | 中国石油化工股份有限公司 | Method of recovering noble metal from spent catalyst containing noble metal |
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| CN107075610A (en) * | 2014-11-10 | 2017-08-18 | 贺利氏德国有限两合公司 | The method that noble metal is removed from the body of formed catalyst containing noble metal |
| CN105944768A (en) * | 2016-05-10 | 2016-09-21 | 能特科技有限公司 | Method for recovering rhodium catalyst from rhodium-containing wastewater |
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