CN115216632A - Platinum and palladium furnace powder refining and purifying process - Google Patents
Platinum and palladium furnace powder refining and purifying process Download PDFInfo
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- CN115216632A CN115216632A CN202210873777.3A CN202210873777A CN115216632A CN 115216632 A CN115216632 A CN 115216632A CN 202210873777 A CN202210873777 A CN 202210873777A CN 115216632 A CN115216632 A CN 115216632A
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Abstract
The invention discloses a platinum and palladium furnace powder refining and purifying process, relates to the technical field of platinum and palladium furnace powder refining, and aims at solving the problem of low recovery rate of the existing platinum and palladium furnace powder purification, the following scheme is proposed, and the scheme comprises the following steps: s1: adding platinum and palladium furnace powder into a reaction device, and then adding hydrochloric acid to ensure that the liquid-solid ratio (4-5) in the reaction device is 1 until the solid is completely dissolved; s2: heating the solution to over 85 ℃, introducing chlorine gas, precipitating platinum and palladium in the form of ammonium chloroplatinate and ammonium chloropalladate, cooling to room temperature, filtering, and washing the co-precipitate of the ammonium chloroplatinate and the ammonium chloropalladate with 10% saturated solution of ammonium chloride for 4-5 times; s3: and then adding water into the co-precipitate, adding water according to a liquid-solid ratio (3-4): 1, boiling for 2 hours to completely dissolve ammonium chloropalladate into the solution, filtering, purifying palladium from filtrate, and purifying platinum from filter residues.
Description
Technical Field
The invention relates to the technical field of platinum and palladium furnace powder refining, in particular to a platinum and palladium furnace powder refining and purifying process.
Background
Platinum and palladium have wide application in various fields of aviation, aerospace, navigation, missiles, rockets, atomic energy, microelectronic technology, chemical engineering, petrochemical industry, glass fiber, waste gas purification and metallurgical industry, become important materials of modern industry, military industry and high-tech industry, and are called as modern industrial vitamins.
In general, in the production of platinum and palladium, the platinum and palladium furnace powder is refined and purified by utilizing a chemical reaction, so that the platinum and the palladium are stored in a simple substance form.
Disclosure of Invention
The invention provides a refining and purifying process of platinum and palladium furnace powder, which solves the problem of low purification and recovery rate of platinum and palladium in the platinum and palladium furnace powder.
In order to achieve the purpose, the invention adopts the following technical scheme:
a platinum and palladium furnace powder refining and purifying process comprises the following steps:
s1: adding platinum and palladium furnace powder into a reaction device, then adding hydrochloric acid, wherein the concentration of the hydrochloric acid is 2 mol/L, so that the liquid-solid ratio (4-5) in the reaction device is 1, the reaction temperature is controlled to be 80-85 ℃, and the reaction is carried out for 4 hours until the solid is completely dissolved;
s2: heating the solution to above 85 ℃, introducing chlorine gas in the reaction process to control the potential to be 390-410 mV, precipitating platinum and palladium in the form of ammonium chloroplatinate and ammonium chloropalladate, cooling to room temperature, filtering, washing the coprecipitate of the ammonium chloroplatinate and the ammonium chloropalladate by using 10% ammonium chloride saturated solution for 4-5 times, and washing impurities;
s3: because the solubility of the ammonium chloroplatinate and the ammonium chloroplatinate in water are different, adding water into a mixture of the ammonium chloroplatinate and the ammonium chloroplatinate according to a liquid-solid ratio (3-4): 1, boiling for 2 hours to completely dissolve the ammonium chloroplatinate in the solution, filtering, purifying palladium from filtrate, and purifying platinum from filter residues;
s4: refining of platinum
Taking the filter residue treated in the step S3, slowly adding aqua regia according to a liquid-solid ratio (2-3): 1, controlling the temperature at 85-90 ℃, reacting for 3 hours, filtering after reaction, removing nitric acid from the filtrate, evaporating the filtrate to be pasty, adding concentrated hydrochloric acid, removing nitre for 2-3 times, finally adding 1% of dilute hydrochloric acid, boiling and dissolving, heating and boiling for a period of time, adding ammonium chloride until no yellow precipitate is generated, then rapidly cooling with circulating cooling water, cooling to room temperature, filtering, and filtering; washing the filter residue with 10% ammonium chloride solution for 4-5 times, repeating the steps for 3-4 times to obtain pure ammonium chloroplatinate, drying the pure ammonium chloroplatinate, calcining in a muffle furnace, controlling the initial calcining temperature at 220-250 ℃, keeping the temperature for 2 h, then heating to 400-450 ℃, keeping the temperature for 1-2 h, then heating to 750 ℃, keeping the temperature for 2-3 h, and slowly cooling to obtain light gray spongy platinum;
s5: refining of Palladium
Taking the filtrate treated in the step S3, heating to over 85 ℃, slowly adding an oxidant and ammonium chloride until no red precipitate is generated, filtering after the reaction is finished, wherein the filtrate is light yellow, washing filter residues by using a 10% ammonium chloride solution, adding water into ammonium chloropalladate, boiling for 2 hours to completely dissolve the ammonium chloropalladate, cooling and filtering, continuously precipitating palladium in the filtrate, precipitating palladium by using ammonium chloride and repeating the water dissolving process for 1-2 times, wherein common metals can be effectively removed in the process, pure ammonium chloropalladate is finally obtained, adding water into the pure ammonium chloropalladate according to the liquid-solid ratio (3-4): 1 for slurrying, adding concentrated ammonia water for adjusting the pH value to 8-9, heating to 80 ℃, supplementing ammonia water in the reaction process, maintaining the pH value of the solution to be 8-9, reacting for 1 hour, cooling and filtering, slowly adding concentrated hydrochloric acid into the ammonia complex solution until the pH value is 1, otherwise, adding water into the solution for slowly adding hydrazine hydrate, controlling the pH value to be higher than that of the sponge, adding water into the hydrazine hydrate solution for controlling the hydration temperature to be higher than that of the pure diamine, heating to be higher than that of the filter residues, drying, and filtering, and adding water to obtain the pure hydrazine hydrate, and drying the diamine with the diamine, and drying the diamine with the temperature of 50-4 ℃ after the temperature is controlled, and drying.
Preferably, the reaction device used in the step S1 includes a reaction kettle, a stirring mechanism is arranged on the inner side of the reaction kettle, an air outlet mechanism is arranged at the bottom of the stirring mechanism, a feeding mechanism which is matched with the stirring mechanism and used for intermittent feeding is arranged on the upper side of the reaction kettle, and a shaking mechanism is arranged on two outer sides of the reaction kettle.
Preferably, rabbling mechanism includes rotates the transmission cover of being connected with the inboard vertical direction of reation kettle, reation kettle's upside fixedly connected with driving motor, driving motor's output fixedly connected with driving gear, one side meshing of driving gear has the driven gear who cup joints with the transmission cover outside is fixed, the downside level of transmission cover rotates and is connected with a plurality of horizontal poles that are located reation kettle inside, and is a plurality of the montant of a plurality of vertical settings of outside fixedly connected with of horizontal pole, a plurality of crushing teeth of the outer fixed surface of montant is connected with, and is a plurality of the one end of horizontal pole is all fixed cup jointed and is located the inboard second bevel gear of transmission cover, the inboard activity of transmission cover is provided with the dead lever with the inboard bottom fixed connection of reation kettle, fixed cup joint on the dead lever have a plurality ofly with the first bevel gear of second bevel gear meshing, the horizontal pole all is provided with the heating pipe with the inboard of montant.
Preferably, the mechanism of giving vent to anger includes the cover of giving vent to anger with dead lever lower extreme fixed connection, the air inlet chamber with the cover intercommunication of giving vent to anger is seted up to the inboard of dead lever, the equal fixedly connected with spring in the inboard both ends of the cover of giving vent to anger, two the slider of the equal fixedly connected with of one end of spring and the inside sliding connection of cover of giving vent to anger, the upside of the cover of giving vent to anger is seted up and is put the venthole with slider complex.
Preferably, feed mechanism include with reation kettle upside fixed connection's raw material tank, the lower extreme intercommunication of raw material tank has the inlet pipe with reation kettle upside intercommunication, the intermediate junction of inlet pipe has the stop collar, the inboard rotation of stop collar is connected with the swing pinion, set up on the swing pinion with inlet pipe complex unloading hole, one side meshing of swing pinion has the intermediate gear with driven gear meshing, the fixed stirring support of being connected with the inboard rotation of raw material tank that has cup jointed in center of swing pinion.
Preferably, rock the mechanism and include with the activity of the reation kettle outside a plurality of bracing pieces that set up, it is a plurality of the equal fixedly connected with uide bushing in upper end of bracing piece, the inboard sliding connection of uide bushing has the arc rack with reation kettle lateral wall fixed connection, the top fixedly connected with accommodate motor of bracing piece, accommodate motor's output fixedly connected with and arc rack toothing's adjusting gear.
Preferably, it is a plurality of the equal fixedly connected with of one end that the transmission cover was kept away from to the horizontal pole sets up with the activity of reation kettle inside wall second scraper blade, the connecting rod that a plurality of slopes of lower extreme fixedly connected with of transmission cover set up, and is a plurality of the equal fixedly connected with of lower extreme of connecting rod slides the first scraper blade that sets up with reation kettle inboard bottom.
Preferably, the upside of reation kettle is provided with feed liquor pipe and blast pipe, reation kettle's bottom is provided with the drain pipe, the upper end of drain pipe is provided with the filter screen, reation kettle's bottom one side has still seted up the discharge opening, reation kettle's the outside be provided with discharge opening complex discharge gate.
The invention has the beneficial effects that:
1. the driving gear is driven to rotate by the driving motor, the transmission sleeve is driven to rotate by the driven gear, a plurality of transverse rods on the transmission sleeve rotate on the inner side of the reaction kettle, the second bevel gears at one ends of the transverse rods are meshed with the first bevel gears on the fixed rods simultaneously, the transverse rods can rotate around the transmission sleeve and can automatically transmit simultaneously, platinum inside the reaction kettle can be driven, palladium furnace powder and hydrochloric acid fully react, the reaction rate is improved, the time required by purification is further reduced, follow-up purification can be improved, the recovery rate is driven when the transverse rods rotate, the stirring range is larger, the reaction rate is further improved, and when the transverse rods rotate, the second scraper at one end of the transverse rods is driven to rotate on the inner side wall of the reaction kettle, the transmission sleeve drives the connecting rod and the first scraper to rotate at the bottom of the reaction kettle, the inner side wall of the reaction kettle and the platinum adhered to the bottom of the reaction kettle are cleaned, the palladium furnace powder is reacted with the hydrochloric acid, and the platinum inside of the reaction kettle is fully reacted with the hydrochloric acid, so that the platinum and the palladium furnace powder is completely dissolved and the follow-up purification treatment is facilitated.
2. Through driven gear, can also drive the idler gear and rotate, and then make the inboard rotary gear of stop collar rotate, make the last unloading hole intermittent type formula of seting up of rotary gear with the inlet pipe cooperation, and then make the inside platinum of raw material tank, in the middle of the reation kettle is entered into to palladium stove powder intermittent type formula, prevent that disposable whole from pouring into reation kettle into, prevent the reaction not thorough, through the blast pipe, can make the poor hydrogen of living of reaction collect, convenient follow-up utilization, prevent that hydrogen is extravagant, through smashing the tooth, can be in the stirring, can be so that the platinum of large granule, palladium stove powder is broken, be convenient for react with hydrochloric acid, the reaction rate is improved, and the steam generator is simple in operation and convenient to use.
Drawings
FIG. 1 is a schematic sectional view of a platinum and palladium furnace powder refining and purifying process according to the present invention;
FIG. 2 is an enlarged schematic view of the refining and purifying process of platinum and palladium furnace powders at A point in the invention;
FIG. 3 is an enlarged schematic view of the point B of the refining and purifying process of the platinum and palladium furnace powder provided by the invention;
FIG. 4 is an enlarged schematic view of the point C of the refining and purifying process of the platinum and palladium furnace powder provided by the invention;
fig. 5 is an enlarged schematic view of a rotating gear in a top view in the refining and purifying process of platinum and palladium furnace powder provided by the invention.
Reference numbers in the figures: 1. a reaction kettle; 2. a transmission sleeve; 3. a liquid inlet pipe; 4. a driving gear; 5. a drive motor; 6. a driven gear; 7. a raw material tank; 8. an exhaust pipe; 9. an adjusting gear; 10. adjusting the motor; 11. a guide sleeve; 12. an arc-shaped rack; 13. a support bar; 14. a discharge door; 15. a liquid outlet pipe; 16. a connecting rod; 17. a first squeegee; 18. a fixing rod; 19. a second squeegee; 20. an intermediate gear; 21. a limiting sleeve; 22. a rotating gear; 23. a blanking hole; 24. a feeding pipe; 25. stirring the bracket; 26. a discharge opening; 27. a slider; 28. a spring; 29. an air outlet sleeve; 30. an air outlet; 31. a first bevel gear; 32. a second bevel gear; 33. heating a tube; 34. a cross bar; 35. crushing teeth; 36. a vertical rod.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1-5, a platinum and palladium furnace powder refining and purifying process comprises the following steps:
s1: adding platinum and palladium furnace powder into a reaction device, then adding hydrochloric acid, wherein the concentration of the hydrochloric acid is 2 mol/L, the liquid-solid ratio (4-5) in the reaction device is 1, the reaction temperature is controlled to be 80-85 ℃, and the reaction is carried out for 4h until the solid is completely dissolved;
s2: heating the solution to above 85 ℃, introducing chlorine gas in the reaction process to control the potential to be 390-410 mV, precipitating platinum and palladium in the forms of ammonium chloroplatinate and ammonium chloropalladate, cooling to room temperature, filtering, washing the co-precipitate of the ammonium chloroplatinate and the ammonium chloropalladate by using a 10% ammonium chloride saturated solution for 4-5 times, and washing impurities;
s3: because the solubility of the ammonium chloroplatinate and the ammonium chloroplatinate in water are different, adding water into a mixture of the ammonium chloroplatinate and the ammonium chloroplatinate according to a liquid-solid ratio (3-4): 1, boiling for 2 hours to completely dissolve the ammonium chloroplatinate in the solution, filtering, purifying palladium from filtrate, and purifying platinum from filter residues;
s4: refining of platinum
Taking the filter residue treated in the step S3, slowly adding aqua regia according to a liquid-solid ratio (2-3): 1, controlling the temperature at 85-90 ℃, reacting for 3 hours, filtering after reaction, removing nitric acid from the filtrate, evaporating the filtrate to be pasty, adding concentrated hydrochloric acid, removing nitre for 2-3 times, finally adding 1% of dilute hydrochloric acid, boiling and dissolving, heating and boiling for a period of time, adding ammonium chloride until no yellow precipitate is generated, then rapidly cooling with circulating cooling water, cooling to room temperature, filtering, and filtering; washing the filter residue with 10% ammonium chloride solution for 4-5 times, repeating the steps for 3-4 times to obtain pure ammonium chloroplatinate, drying the pure ammonium chloroplatinate, calcining in a muffle furnace, controlling the initial calcining temperature at 220-250 ℃, keeping the temperature for 2 h, then heating to 400-450 ℃, keeping the temperature for 1-2 h, then heating to 750 ℃, keeping the temperature for 2-3 h, and slowly cooling to obtain light gray spongy platinum;
s5: refining of palladium
Taking the filtrate treated in the step S3, heating to over 85 ℃, slowly adding an oxidant and ammonium chloride until no red precipitate is generated, filtering after the reaction is finished, wherein the filtrate is light yellow, washing filter residues by using a 10% ammonium chloride solution, adding water into ammonium chloropalladate, boiling for 2 hours to completely dissolve the ammonium chloropalladate, cooling and filtering, continuously precipitating palladium in the filtrate, precipitating palladium by using ammonium chloride and repeating the water dissolving process for 1-2 times, wherein common metals can be effectively removed in the process, pure ammonium chloropalladate is finally obtained, adding water into the pure ammonium chloropalladate according to the liquid-solid ratio (3-4): 1 for slurrying, adding concentrated ammonia water for adjusting the pH value to 8-9, heating to 80 ℃, supplementing ammonia water in the reaction process, maintaining the pH value of the solution to be 8-9, reacting for 1 hour, cooling and filtering, slowly adding concentrated hydrochloric acid into the ammonia complex solution until the pH value is 1, otherwise, adding water into the solution for slowly adding hydrazine hydrate, controlling the pH value to be higher than that of the sponge, adding water into the hydrazine hydrate solution for controlling the hydration temperature to be higher than that of the pure diamine, heating to be higher than that of the filter residues, drying, and filtering, and adding water to obtain the pure hydrazine hydrate, and drying the diamine with the diamine, and drying the diamine with the temperature of 50-4 ℃ after the temperature is controlled, and drying.
The reaction device used in the step S1 comprises a reaction kettle 1, wherein a stirring mechanism is arranged on the inner side of the reaction kettle 1, an air outlet mechanism is arranged at the bottom of the stirring mechanism, a feeding mechanism which is matched with the stirring mechanism and used for intermittent feeding is arranged on the upper side of the reaction kettle 1, shaking mechanisms are arranged on two outer sides of the reaction kettle 1, the stirring mechanism comprises a transmission sleeve 2 which is rotatably connected with the inner side of the reaction kettle 1 in the vertical direction, a driving motor 5 is fixedly connected with the upper side of the reaction kettle 1, a driving gear 4 is fixedly connected with the output end of the driving motor 5, a driven gear 6 which is fixedly sleeved with the outer side of the transmission sleeve 2 is meshed with one side of the driving gear 4, a plurality of transverse rods 34 which are positioned inside the reaction kettle 1 are horizontally and rotatably connected with the lower side of the transmission sleeve 2, a plurality of vertical rods 36 which are vertically arranged are fixedly connected with the outer sides of the plurality of transverse rods 34, and a plurality of crushing teeth 35 are fixedly connected with the outer surfaces of the vertical rods 36, one end of each of a plurality of transverse rods 34 is fixedly sleeved with a second bevel gear 32 positioned on the inner side of the transmission sleeve 2, the inner side of the transmission sleeve 2 is movably provided with a fixed rod 18 fixedly connected with the bottom of the inner side of the reaction kettle 1, the fixed rod 18 is fixedly sleeved with a plurality of first bevel gears 31 meshed with the second bevel gears 32, the inner sides of the transverse rods 34 and the vertical rods 36 are respectively provided with a heating pipe 33, the air outlet mechanism comprises an air outlet sleeve 29 fixedly connected with the lower end of the fixed rod 18, the inner side of the fixed rod 18 is provided with an air inlet cavity communicated with the air outlet sleeve 29, both ends of the inner side of the air outlet sleeve 29 are respectively and fixedly connected with springs 28, one end of each of the two springs 28 is respectively and fixedly connected with a sliding block 27 slidably connected with the inner side of the air outlet sleeve 29, the upper side of the air outlet sleeve 29 is provided with an air outlet hole 30 matched with the sliding block 27, the feeding mechanism comprises a raw material box 7 fixedly connected with the upper side of the reaction kettle 1, the lower end of the raw material box 7 is communicated with a feeding pipe 24 communicated with the upper side of the reaction kettle 1, the middle of the feeding pipe 24 is connected with a limiting sleeve 21, the inner side of the limiting sleeve 21 is rotatably connected with a rotary gear 22, a blanking hole 23 matched with the feeding pipe 24 is formed in the rotary gear 22, one side of the rotary gear 22 is meshed with an intermediate gear 20 meshed with a driven gear 6, a stirring support 25 rotatably connected with the inner side of the raw material box 7 is fixedly sleeved in the center of the rotary gear 22, platinum and palladium furnace powder is poured into the raw material box 7, hydrochloric acid is added into the reaction kettle 1 through a liquid inlet pipe 3, then a driving motor 5 drives a transmission sleeve 2 to rotate through a driving gear 4 and the driven gear 6, meanwhile, the driven gear 6 drives the intermediate gear 20 to rotate, the rotary gear 22 rotates, the blanking hole 23 in the rotary gear 22 is intermittently matched with the feeding pipe 24, and the platinum and palladium furnace powder inside the raw material box 7 intermittently flows into the reaction kettle 1, the platinum and palladium furnace powder reacts with the hydrochloric acid in batches, so that the reaction is more sufficient, the reaction rate is improved, the stirring support 25 is driven to rotate in the raw material box 7 while the intermediate gear 20 rotates, the platinum and palladium furnace powder can rapidly enter the feeding pipe 24 and further flow into the reaction kettle 1, the feeding pipe 24 is prevented from being blocked by the platinum and palladium furnace powder to influence the feeding of the platinum and palladium furnace powder, the platinum and palladium furnace powder and the hydrochloric acid can be stirred through the rotation of the cross rod 34 and the vertical rod 36, the reaction rate is further improved, the temperature of the solution in the reaction kettle 1 can be increased through the heating pipes 33 in the cross rod 34 and the vertical rod 36, the reaction temperature is initially controlled to be 80-85 ℃, the reaction rate of the platinum, palladium furnace powder and the hydrochloric acid can be fastest, and the temperature of the solution can be rapidly improved, the time for subsequently purifying platinum and palladium from platinum and palladium furnace powder is reduced, when the platinum and palladium furnace powder is completely dissolved in hydrochloric acid, the air inlet cavity formed in the fixing rod 18 is utilized, chlorine is pumped into the fixing rod 18 through the upper end of the fixing rod 18 and flows into the air outlet sleeve 29, then the sliding block 27 on the inner side of the air outlet sleeve 29 is pressed to compress the spring 28, the sliding block 27 opens the air outlet hole 30 on the upper side of the air outlet sleeve 29, chlorine enters the reaction kettle 1 through the air outlet hole 30, meanwhile, the temperature of the solution is increased to more than 85 ℃ through the heating pipe 33, platinum and palladium in the solution can be precipitated in the form of ammonium chloroplatinate and then cooled to room temperature.
Rocking mechanism includes a plurality of bracing pieces 13 with the activity setting in the 1 outside of reation kettle, the equal fixedly connected with uide bushing 11 in upper end of a plurality of bracing pieces 13, the inboard sliding connection of uide bushing 11 has arc rack 12 with 1 lateral wall fixed connection of reation kettle, the top fixedly connected with accommodate motor 10 of bracing piece 13, the output fixedly connected with of accommodate motor 10 and the adjusting gear 9 of arc rack 12 meshing, drive accommodate gear 9 through accommodate motor 10 and rotate, and then make arc rack 12 rotate, make reation kettle 1 can the reciprocating swing about, make mixed liquid stirring more abundant in reation kettle 1, and when the discharge precipitate, can make reation kettle 1 rotate certain angle, make the discharge opening be in the lower, conveniently make the precipitate discharge of reation kettle 1 inside fast, improve the speed of unloading.
The equal fixedly connected with of one end of transmission cover 2 and the second scraper blade 19 that the activity of 1 inside wall of reation kettle set up are kept away from to a plurality of horizontal poles 34, the connecting rod 16 that the lower extreme fixedly connected with of transmission cover 2 set up with the connecting rod 16 of the activity of 1 inside wall of reation kettle, the equal fixedly connected with of lower extreme of a plurality of connecting rods 16 slides the first scraper blade 17 that sets up with the inboard bottom of reation kettle, through first scraper blade 17 and second scraper blade 19, can be so that the platinum on 1 inside wall of reation kettle and the bottom, palladium stove powder strikes off, make it fully react with hydrochloric acid, make platinum, palladium stove powder dissolve in the middle of hydrochloric acid fast, follow-up platinum can be improved, the purification rate of recovery of palladium, high durability and convenient use.
The working principle is as follows: platinum and palladium furnace powder is poured into a raw material box 7, hydrochloric acid is added into a reaction kettle 1 through a liquid inlet pipe 3, a driving motor 5 drives a transmission sleeve 2 to rotate through a driving gear 4 and a driven gear 6, meanwhile, the driven gear 6 drives an intermediate gear 20 to rotate, a rotary gear 22 is made to rotate, a blanking hole 23 on the rotary gear 22 is made to be intermittently matched with a feeding pipe 24, platinum and palladium furnace powder inside the raw material box 7 flows into the reaction kettle 1 intermittently, the platinum and palladium furnace powder reacts with the hydrochloric acid in batches, therefore, the reaction is more sufficient, the reaction rate is improved, and a stirring support 25 is driven to rotate inside the raw material box 7 while the intermediate gear 20 rotates, so that the platinum and palladium furnace powder can more rapidly enter the feeding pipe 24 and then flows into the reaction kettle 1, the platinum and palladium furnace powder is prevented from blocking the feeding pipe 24, the feeding of the platinum and palladium furnace powders is influenced, the platinum and palladium furnace powders and the hydrochloric acid can be stirred through the rotation of the cross rod 34 and the vertical rod 36, the reaction rate is further improved, the temperature of the solution in the reaction kettle 1 can be increased through the heating pipe 33 in the cross rod 34 and the vertical rod 36, the reaction temperature is controlled to be 80-85 ℃ at the beginning, the reaction rate of the platinum and palladium furnace powders and the hydrochloric acid is fastest, the temperature of the solution is also conveniently and rapidly increased, the time for subsequently purifying the platinum and palladium from the platinum and palladium furnace powders is reduced, when the platinum and palladium furnace powders are completely dissolved in the hydrochloric acid, chlorine is pumped into the fixing rod 18 through the upper end of the fixing rod 18 through the air inlet cavity formed in the fixing rod 18 and then flows into the air outlet sleeve 29, then the sliding block 27 on the inner side of the air outlet sleeve 29 is pressed to compress the spring 28, make slider 27 open the venthole 30 of gas pocket 29 upside, and then make chlorine enter into reation kettle 1 in the middle of through venthole 30, simultaneously through heating pipe 33, make the temperature of solution rise to more than 85 ℃, can make platinum in the middle of the solution, palladium is with chloroplatinic acid ammonium, chloroplatinic acid ammonium's form deposits, then cool to room temperature, discharge liquid through drain pipe 15 after that, make the precipitate discharge through discharge opening 26, just can carry out subsequent purification process, further shorten the required time of purification, drive adjusting gear 9 through adjusting motor 10 and rotate, and then make arc rack 12 rotate, make reation kettle 1 can left and right sides reciprocal swing, make mixed liquid stirring more abundant in reation kettle 1, and when discharging the precipitate, can make reation kettle 1 rotate certain angle, make the discharge opening be in the lowest, conveniently make the inside precipitate of reation kettle 1 discharge fast, improve the speed of unloading.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations or positional relationships based on those shown in the drawings, merely for convenience of description and simplicity of description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A platinum and palladium furnace powder refining and purifying process is characterized by comprising the following steps:
s1: adding platinum and palladium furnace powder into a reaction device, then adding hydrochloric acid, wherein the concentration of the hydrochloric acid is 2 mol/L, the liquid-solid ratio (4-5) in the reaction device is 1, the reaction temperature is controlled to be 80-85 ℃, and the reaction is carried out for 4h until the solid is completely dissolved;
s2: heating the solution to above 85 ℃, introducing chlorine gas in the reaction process to control the potential to be 390-410 mV, precipitating platinum and palladium in the form of ammonium chloroplatinate and ammonium chloropalladate, cooling to room temperature, filtering, washing the coprecipitate of the ammonium chloroplatinate and the ammonium chloropalladate by using 10% ammonium chloride saturated solution for 4-5 times, and washing impurities;
s3: because the solubility of the ammonium chloroplatinate and the ammonium chloroplatinate in water are different, adding water into a mixture of the ammonium chloroplatinate and the ammonium chloroplatinate according to a liquid-solid ratio (3-4): 1, boiling for 2 hours to completely dissolve the ammonium chloroplatinate in the solution, filtering, purifying palladium from filtrate, and purifying platinum from filter residues;
s4: refining of platinum
Taking the filter residue treated in the step S3, slowly adding aqua regia according to a liquid-solid ratio (2-3): 1, controlling the temperature at 85-90 ℃, reacting for 3 hours, filtering after reaction, removing nitric acid from the filtrate, evaporating the filtrate to be pasty, adding concentrated hydrochloric acid, removing nitre for 2-3 times, finally adding 1% of dilute hydrochloric acid, boiling and dissolving, heating and boiling for a period of time, adding ammonium chloride until no yellow precipitate is generated, then rapidly cooling with circulating cooling water, cooling to room temperature, filtering, and filtering; washing the filter residue with 10% ammonium chloride solution for 4-5 times, repeating the washing for 3-4 times, and finally obtaining pure ammonium chloroplatinate, drying the pure ammonium chloroplatinate, calcining in a muffle furnace, controlling the initial calcining temperature at 220-250 ℃, keeping the temperature for 2 hours, then heating to 400-450 ℃, keeping the temperature for 1-2 hours, then heating to 750 ℃, keeping the temperature for 2-3 hours, and slowly cooling to obtain light gray spongy platinum;
s5: refining of palladium
Taking the filtrate treated in the step S3, heating to over 85 ℃, slowly adding an oxidant and ammonium chloride until no red precipitate is generated, filtering after the reaction is finished, wherein the filtrate is light yellow, washing filter residues by using a 10% ammonium chloride solution, adding water into ammonium chloropalladate, boiling for 2 hours to completely dissolve the ammonium chloropalladate, cooling and filtering, continuously precipitating palladium in the filtrate, precipitating palladium by using ammonium chloride and repeating the water dissolving process for 1-2 times, wherein common metals can be effectively removed in the process, pure ammonium chloropalladate is finally obtained, adding water into the pure ammonium chloropalladate according to the liquid-solid ratio (3-4): 1 for slurrying, adding concentrated ammonia water for adjusting the pH value to 8-9, heating to 80 ℃, supplementing ammonia water in the reaction process, maintaining the pH value of the solution to be 8-9, reacting for 1 hour, cooling and filtering, slowly adding concentrated hydrochloric acid into the ammonia complex solution until the pH value is 1, otherwise, adding water into the solution for slowly adding hydrazine hydrate, controlling the pH value to be higher than that of the sponge, adding water into the hydrazine hydrate solution for controlling the hydration temperature to be higher than that of the pure diamine, heating to be higher than that of the filter residues, drying, and filtering, and adding water to obtain the pure hydrazine hydrate, and drying the diamine with the diamine, and drying the diamine with the temperature of 50-4 ℃ after the temperature is controlled, and drying.
2. The platinum and palladium furnace powder refining and purifying process according to claim 1, wherein the reaction device used in the step S1 comprises a reaction kettle (1), a stirring mechanism is arranged inside the reaction kettle (1), an air outlet mechanism is arranged at the bottom of the stirring mechanism, a feeding mechanism which is used for intermittent feeding and is matched with the stirring mechanism is arranged on the upper side of the reaction kettle (1), and shaking mechanisms are arranged on two outer sides of the reaction kettle (1).
3. The refining and purifying process of the platinum and palladium furnace powder as claimed in claim 2, wherein the stirring mechanism comprises a transmission sleeve (2) rotatably connected with the inner side of the reaction kettle (1) in the vertical direction, the upper side of the reaction kettle (1) is fixedly connected with a driving motor (5), an output end of the driving motor (5) is fixedly connected with a driving gear (4), one side of the driving gear (4) is engaged with a driven gear (6) fixedly sleeved with the outer side of the transmission sleeve (2), the lower side of the transmission sleeve (2) is horizontally and rotatably connected with a plurality of transverse rods (34) positioned inside the reaction kettle (1), a plurality of vertical rods (36) fixedly connected with a plurality of vertical arrangements are fixedly connected with the outer side of the transverse rods (34), a plurality of crushing teeth (35) are fixedly connected with the outer surface of the vertical rods (36), a plurality of second bevel gears (32) positioned inside the transmission sleeve (2) are fixedly sleeved with one end of the transverse rods (34), the inner side of the transmission sleeve (2) is movably provided with fixing rods (18) fixedly connected with the inner side of the bottom of the reaction kettle (1), a plurality of transverse rods (18) are connected with a plurality of bevel gears (32) engaged with the transverse rods (31), and a first bevel gear (33) is connected with the inner side of the transverse rod (34), and a heating pipe (33) is movably arranged on the fixing sleeve (18).
4. The refining and purifying process of the platinum and palladium furnace powder as claimed in claim 3, wherein the air outlet mechanism comprises an air outlet sleeve (29) fixedly connected with the lower end of a fixing rod (18), an air inlet cavity communicated with the air outlet sleeve (29) is formed in the inner side of the fixing rod (18), springs (28) are fixedly connected to both ends of the inner side of the air outlet sleeve (29), a sliding block (27) slidably connected with the inner side of the air outlet sleeve (29) is fixedly connected to one end of each of the two springs (28), and an air outlet hole (30) matched with the sliding block (27) is formed in the upper side of the air outlet sleeve (29).
5. The platinum and palladium furnace powder refining and purifying process according to claim 3, wherein the feeding mechanism comprises a raw material box (7) fixedly connected with the upper side of the reaction kettle (1), the lower end of the raw material box (7) is communicated with a feeding pipe (24) communicated with the upper side of the reaction kettle (1), the middle of the feeding pipe (24) is connected with a limiting sleeve (21), the inner side of the limiting sleeve (21) is rotatably connected with a rotating gear (22), the rotating gear (22) is provided with a feeding hole (23) matched with the feeding pipe (24), one side of the rotating gear (22) is engaged with an intermediate gear (20) engaged with the driven gear (6), and the center of the rotating gear (22) is fixedly sleeved with a stirring support (25) rotatably connected with the inner side of the raw material box (7).
6. The refining and purifying process of the platinum and palladium furnace powder as claimed in claim 1, wherein the shaking mechanism comprises a plurality of support rods (13) movably arranged outside the reaction kettle (1), the upper ends of the plurality of support rods (13) are fixedly connected with guide sleeves (11), the inner sides of the guide sleeves (11) are slidably connected with arc-shaped racks (12) fixedly connected with the side walls of the reaction kettle (1), the top ends of the support rods (13) are fixedly connected with adjusting motors (10), and the output ends of the adjusting motors (10) are fixedly connected with adjusting gears (9) meshed with the arc-shaped racks (12).
7. The platinum and palladium furnace powder refining and purifying process according to claim 3, characterized in that one end of each of the plurality of cross rods (34) far away from the transmission sleeve (2) is fixedly connected with a second scraper (19) movably arranged on the inner side wall of the reaction kettle (1), the lower end of the transmission sleeve (2) is fixedly connected with a plurality of obliquely arranged connecting rods (16), and the lower end of each of the plurality of connecting rods (16) is fixedly connected with a first scraper (17) slidably arranged on the bottom of the inner side of the reaction kettle (1).
8. The platinum and palladium furnace powder refining and purifying process according to claim 2, characterized in that a liquid inlet pipe (3) and an exhaust pipe (8) are arranged on the upper side of the reaction kettle (1), a liquid outlet pipe (15) is arranged at the bottom of the reaction kettle (1), a filter screen is arranged at the upper end of the liquid outlet pipe (15), a discharge opening (26) is further formed in one side of the bottom of the reaction kettle (1), and a discharge door (14) matched with the discharge opening (26) is arranged on the outer side of the reaction kettle (1).
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| GB863286A (en) * | 1958-02-04 | 1961-03-22 | Canadian Copper Refiners Ltd | Improvements in or relating to processes of separating palladium from metals of the platinum group |
| KR910005057B1 (en) * | 1988-08-19 | 1991-07-22 | 방세훈 | Method for refining of pt,pd |
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| CN107051433A (en) * | 2017-03-08 | 2017-08-18 | 华东理工大学 | The preparation method of zinc oxide supported palladium/platinum catalyst and the application in CO catalysis oxidations |
| CN110512091A (en) * | 2019-09-19 | 2019-11-29 | 李旭意 | It is a kind of using ammonium chloropalladate as the palladium method of refining of raw material |
| CN110964917A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Palladium refining process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB863286A (en) * | 1958-02-04 | 1961-03-22 | Canadian Copper Refiners Ltd | Improvements in or relating to processes of separating palladium from metals of the platinum group |
| KR910005057B1 (en) * | 1988-08-19 | 1991-07-22 | 방세훈 | Method for refining of pt,pd |
| JP2003027154A (en) * | 2001-07-18 | 2003-01-29 | Nikko Materials Co Ltd | Method of recovering high-purity platinum and palladium |
| CN105112681A (en) * | 2015-09-07 | 2015-12-02 | 山东恒邦冶炼股份有限公司 | Method for extracting gold platinum and palladium from platinum and palladium concentrate |
| CN107051433A (en) * | 2017-03-08 | 2017-08-18 | 华东理工大学 | The preparation method of zinc oxide supported palladium/platinum catalyst and the application in CO catalysis oxidations |
| CN110964917A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Palladium refining process |
| CN110512091A (en) * | 2019-09-19 | 2019-11-29 | 李旭意 | It is a kind of using ammonium chloropalladate as the palladium method of refining of raw material |
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