CN115216632B - Refining and purifying process for platinum and palladium furnace powder - Google Patents
Refining and purifying process for platinum and palladium furnace powder Download PDFInfo
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- CN115216632B CN115216632B CN202210873777.3A CN202210873777A CN115216632B CN 115216632 B CN115216632 B CN 115216632B CN 202210873777 A CN202210873777 A CN 202210873777A CN 115216632 B CN115216632 B CN 115216632B
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- 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
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- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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Abstract
The invention discloses a refining and purifying process of platinum and palladium furnace powder, which 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 refining, and the invention provides the following scheme that the process comprises the following steps: s1: adding platinum and palladium furnace powder into a reaction device, and then adding hydrochloric acid to enable the liquid-solid ratio (4-5) in the reaction device to be 1 until the solid is completely dissolved; s2: then heating the solution to above 85 ℃, then introducing chlorine gas, precipitating platinum and palladium in the form of ammonium chloroplatinate and ammonium chloropalladate, cooling to room temperature, filtering, and washing the ammonium chloroplatinate and ammonium chloropalladate coprecipitate with 10% ammonium chloride saturated solution for 4-5 times; s3: then adding water into the coprecipitate, adding water according to the liquid-solid ratio (3-4): 1, boiling 2 h to make ammonium chloropalladate completely dissolve in the solution, filtering, purifying palladium from filtrate and purifying platinum from filter residue.
Description
Technical Field
The invention relates to the technical field of refining of platinum and palladium furnace powder, in particular to a refining and purifying process of platinum and palladium furnace powder.
Background
Platinum and palladium have wide application in various fields of aviation, aerospace, navigation, missile, rocket, atomic energy, microelectronics, chemical industry, petrochemical industry, glass fiber, waste gas purification and metallurgical industry, and become important materials in modern industry, military industry and high and new technology industry, and are called as 'modern industrial vitamins'.
In general, the production of platinum and palladium makes the platinum and palladium furnace powder undergo the process of refining and purification by utilizing chemical reaction, so that the platinum and palladium can be stored in the form of simple substance, and the existing purification process can be used for purifying platinum and palladium, but the purification recovery rate is low, so that the platinum and palladium furnace powder refining and purification process is not popular in production.
Disclosure of Invention
The invention provides a refining and purifying process for platinum and palladium furnace powder, which solves the problem of low recovery rate of platinum and palladium in the platinum and palladium furnace powder.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a refining and purifying process for platinum and palladium furnace powder 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 4h until the solid is completely dissolved;
s2: then heating the solution to above 85 ℃, then introducing chlorine, controlling the potential of the chlorine to 390-410 mV in the reaction process, precipitating platinum and palladium in the form of ammonium chloroplatinate and ammonium chloropalladate, cooling to room temperature, filtering, washing the ammonium chloroplatinate and ammonium chloropalladate coprecipitate for 4-5 times by using 10% ammonium chloride saturated solution, and washing impurities;
s3: because the solubility of ammonium chloroplatinate and ammonium chloropalladate in water is different, adding water into the mixture of ammonium chloroplatinate and ammonium chloropalladate according to the liquid-solid ratio (3-4) of 1, boiling 2 h to completely dissolve the ammonium chloropalladate in the solution, filtering, purifying palladium from the filtrate and purifying platinum from the filter residue;
s4: refining of platinum
Taking filter residues treated in the step S3, slowly adding aqua regia according to the liquid-solid ratio (2-3), controlling the temperature at 85-90 ℃, reacting at 3-h, filtering after the reaction, removing nitric acid from filtrate, evaporating the filtrate to paste, adding concentrated hydrochloric acid, removing nitric acid for 2-3 times again, adding 1% of dilute hydrochloric acid to boil and dissolve, heating and boiling for a period of time, adding ammonium chloride until no yellow precipitate is generated, then rapidly cooling by circulating cooling water, cooling to room temperature, finally filtering, and filtering; washing filter residues 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 constant temperature at 2 h, heating to 400-450 ℃, keeping the constant temperature at 1-2 h, heating to 750 ℃, keeping the constant temperature at 2-3 h, and slowly cooling to obtain light gray sponge platinum;
s5: refining of palladium
And (3) heating the filtrate treated in the step (S3) to above 85 ℃, slowly adding an oxidant and ammonium chloride until no red precipitate is generated, filtering after the reaction is finished, washing filter residues with 10% ammonium chloride solution, adding water into ammonium chloropalladate, boiling 2 for h to completely dissolve the ammonium chloropalladate, cooling and filtering, continuously precipitating palladium from the filtrate, repeating the processes of ammonium chloride palladium precipitation and water dissolution for 1-2 times, effectively removing common metals in the process, finally obtaining pure ammonium chloropalladate, and then mixing the pure ammonium chloropalladate according to a liquid-solid ratio (3-4): 1, adding water for pulping, adding concentrated ammonia water to adjust the pH value to 8-9, heating to 80 ℃, adding ammonia water in the reaction process, maintaining the pH value of the solution to 8-9, reacting to 1-h, cooling and filtering, slowly adding hydrazine hydrate because dichlorotetra-ammine palladium and hydrochloric acid are exothermic reaction, slowly adding concentrated hydrochloric acid into the ammonia water complexing solution until the pH value is 1, otherwise, generating soluble cis-dichlorodi-ammine palladium by excessively high solution temperature, thereby reducing the recovery rate of palladium, controlling the solution temperature to be less than 45 ℃, filtering, washing filter residues with hydrochloric acid with the pH value of 1, complexing ammonia water and acidifying hydrochloric acid for 3-4 times, finally obtaining pure dichlorodiamine palladium, slurrying pure dichlorodiamine palladium with water, heating to 40-50 ℃, slowly adding hydrazine hydrate, adding hydrazine hydrate to be not too fast, otherwise, generating palladium powder particles to be larger, easily bringing out impurity elements to influence the purity of palladium powder, drying palladium powder for 4h at 120 ℃ after washing with water, and obtaining the palladium sponge powder.
Preferably, the reaction device used in the step S1 comprises 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 for intermittent feeding matched with the stirring mechanism is arranged on the upper side of the reaction kettle, and shaking mechanisms are arranged on two sides of the outer part of the reaction kettle.
Preferably, the stirring mechanism comprises a transmission sleeve which is rotationally connected with the inner side of the reaction kettle in the vertical direction, a driving motor is fixedly connected to the upper side of the reaction kettle, a driving gear is fixedly connected to the output end of the driving motor, a driven gear which is fixedly sleeved on the outer side of the transmission sleeve is meshed with one side of the driving gear, a plurality of transverse rods which are positioned in the reaction kettle are horizontally rotationally connected to the lower side of the transmission sleeve, a plurality of vertical rods which are vertically arranged are fixedly connected to the outer side of the transverse rods, a plurality of crushing teeth are fixedly connected to the outer surface of the vertical rods, a second bevel gear which is positioned on the inner side of the transmission sleeve is fixedly sleeved on one end of the transverse rods, a plurality of first bevel gears which are meshed with the second bevel gear are fixedly sleeved on the fixing rod, and heating pipes are arranged on the inner sides of the transverse rods and the vertical rods.
Preferably, the air outlet mechanism comprises an air outlet sleeve fixedly connected with the lower end of the fixing rod, an air inlet cavity communicated with the air outlet sleeve is formed in the inner side of the fixing rod, springs are fixedly connected to the two ends of the inner side of the air outlet sleeve, a sliding block is fixedly connected to one end of each spring and is in sliding connection with the inner side of the air outlet sleeve, and an air outlet hole matched with the sliding block is formed in the upper side of the air outlet sleeve.
Preferably, the feeding mechanism comprises a raw material box fixedly connected with the upper side of the reaction kettle, a feeding pipe communicated with the upper side of the reaction kettle is communicated with the lower end of the raw material box, a limit sleeve is connected in the middle of the feeding pipe, a rotary gear is rotationally connected with the inner side of the limit sleeve, a discharging hole matched with the feeding pipe is formed in the rotary gear, an intermediate gear meshed with a driven gear is meshed with one side of the rotary gear, and a stirring bracket rotationally connected with the inner side of the raw material box is fixedly sleeved at the center of the rotary gear.
Preferably, the rocking mechanism comprises a plurality of support rods movably arranged on the outer side of the reaction kettle, the upper ends of the support rods are fixedly connected with guide sleeves, the inner sides of the guide sleeves are slidably connected with arc racks fixedly connected with the side walls of the reaction kettle, the top ends of the support rods are fixedly connected with adjusting motors, and the output ends of the adjusting motors are fixedly connected with adjusting gears meshed with the arc racks.
Preferably, a plurality of the horizontal poles keep away from the second scraper blade that the activity of the equal fixedly connected with of one end of transmission cover and reation kettle inside wall set up, the lower extreme fixedly connected with of transmission cover a plurality of slopes set up the connecting rod, a plurality of the equal fixedly connected with of lower extreme of connecting rod and the first scraper blade that the inboard bottom of reation kettle slided and set up.
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, the discharge opening has still been seted up to bottom one side of reation kettle, reation kettle's outside is provided with the door of unloading with discharge opening complex.
The invention has the beneficial effects that:
1. the driving gear is driven to rotate through the driving motor, and then the driving sleeve is driven to rotate through the driven gear, a plurality of cross bars on the driving sleeve rotate on the inner side of the reaction kettle, and meanwhile, the second bevel gears at one ends of the cross bars are meshed with the first bevel gears on the fixing rods, so that the cross bars can be cleaned when rotating around the driving sleeve, and simultaneously self-transmission is carried out, platinum and palladium furnace powder inside the reaction kettle fully react with hydrochloric acid, the reaction rate is improved, the time required by purification is further reduced, the subsequent purification recovery rate can be improved, and when the cross bars rotate, the vertical bars are driven to rotate, so that the stirring range is larger, the reaction rate is further improved, and meanwhile, the second scraping plates at one ends of the cross bars are driven to rotate on the inner side wall of the reaction kettle, the connecting rods are driven by the driving sleeve to rotate with the bottom of the first scraping plates, so that platinum and palladium furnace powder adhered on the inner side wall of the reaction kettle are cleaned, and hydrochloric acid are reacted, the platinum and palladium furnace powder inside the reaction kettle fully react with hydrochloric acid, and the platinum and palladium furnace powder are dissolved completely, and subsequent purification treatment is facilitated.
2. Through driven gear rotation, can also drive intermediate gear rotation, and then make the inboard rotatory gear of stop collar rotate, make the intermittent type formula of unloading hole that sets up on the rotatory gear with the inlet pipe cooperation, and then make the inside platinum of raw materials case, palladium stove powder intermittent type formula enter into reation kettle in the middle of, prevent disposable whole pouring into reation kettle, prevent the incomplete reaction, through the blast pipe, can make the hydrogen that the reaction is bad collect, make things convenient for follow-up utilization, prevent hydrogen extravagant, through crushing tooth, can make the platinum of macroparticle, palladium stove powder break in the stirring, be convenient for react with hydrochloric acid, improve reaction rate, and easy operation, convenient for use.
Drawings
FIG. 1 is a schematic diagram of a platinum and palladium furnace powder refining and purifying process in a front cross-sectional view;
FIG. 2 is an enlarged schematic diagram of the A part of a refining and purifying process of platinum and palladium furnace powder;
FIG. 3 is an enlarged schematic diagram of the refining and purifying process of the platinum and palladium furnace powder at the position B;
FIG. 4 is an enlarged schematic diagram of a refining and purifying process of platinum and palladium furnace powder at C;
fig. 5 is an enlarged schematic diagram of a rotary gear in top view of a refining and purifying process of platinum and palladium furnace powder.
Reference numerals in the drawings: 1. a reaction kettle; 2. a transmission sleeve; 3. a liquid inlet pipe; 4. a drive gear; 5. a driving motor; 6. a driven gear; 7. a raw material box; 8. an exhaust pipe; 9. an adjusting gear; 10. adjusting a motor; 11. a guide sleeve; 12. an arc-shaped rack; 13. a support rod; 14. a discharge door; 15. a liquid outlet pipe; 16. a connecting rod; 17. a first scraper; 18. a fixed rod; 19. a second scraper; 20. an intermediate gear; 21. a limit sleeve; 22. a rotary gear; 23. a blanking hole; 24. a feed pipe; 25. a stirring bracket; 26. a discharge port; 27. a slide block; 28. a spring; 29. an air outlet sleeve; 30. an air outlet hole; 31. a first bevel gear; 32. a second bevel gear; 33. heating pipes; 34. a cross bar; 35. crushing teeth; 36. and a vertical rod.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Referring to fig. 1-5, a refining and purifying process for platinum and palladium furnace powder 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 4h until the solid is completely dissolved;
s2: then heating the solution to above 85 ℃, then introducing chlorine, controlling the potential of the chlorine to 390-410 mV in the reaction process, precipitating platinum and palladium in the form of ammonium chloroplatinate and ammonium chloropalladate, cooling to room temperature, filtering, washing the ammonium chloroplatinate and ammonium chloropalladate coprecipitate for 4-5 times by using 10% ammonium chloride saturated solution, and washing impurities;
s3: because the solubility of ammonium chloroplatinate and ammonium chloropalladate in water is different, adding water into the mixture of ammonium chloroplatinate and ammonium chloropalladate according to the liquid-solid ratio (3-4) of 1, boiling 2 h to completely dissolve the ammonium chloropalladate in the solution, filtering, purifying palladium from the filtrate and purifying platinum from the filter residue;
s4: refining of platinum
Taking filter residues treated in the step S3, slowly adding aqua regia according to the liquid-solid ratio (2-3), controlling the temperature at 85-90 ℃, reacting at 3-h, filtering after the reaction, removing nitric acid from filtrate, evaporating the filtrate to paste, adding concentrated hydrochloric acid, removing nitric acid for 2-3 times again, adding 1% of dilute hydrochloric acid to boil and dissolve, heating and boiling for a period of time, adding ammonium chloride until no yellow precipitate is generated, then rapidly cooling by circulating cooling water, cooling to room temperature, finally filtering, and filtering; washing filter residues 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 constant temperature at 2 h, heating to 400-450 ℃, keeping the constant temperature at 1-2 h, heating to 750 ℃, keeping the constant temperature at 2-3 h, and slowly cooling to obtain light gray sponge platinum;
s5: refining of palladium
And (3) heating the filtrate treated in the step (S3) to above 85 ℃, slowly adding an oxidant and ammonium chloride until no red precipitate is generated, filtering after the reaction is finished, washing filter residues with 10% ammonium chloride solution, adding water into ammonium chloropalladate, boiling 2 for h to completely dissolve the ammonium chloropalladate, cooling and filtering, continuously precipitating palladium from the filtrate, repeating the processes of ammonium chloride palladium precipitation and water dissolution for 1-2 times, effectively removing common metals in the process, finally obtaining pure ammonium chloropalladate, and then mixing the pure ammonium chloropalladate according to a liquid-solid ratio (3-4): 1, adding water for pulping, adding concentrated ammonia water to adjust the pH value to 8-9, heating to 80 ℃, adding ammonia water in the reaction process, maintaining the pH value of the solution to 8-9, reacting to 1-h, cooling and filtering, slowly adding hydrazine hydrate because dichlorotetra-ammine palladium and hydrochloric acid are exothermic reaction, slowly adding concentrated hydrochloric acid into the ammonia water complexing solution until the pH value is 1, otherwise, generating soluble cis-dichlorodi-ammine palladium by excessively high solution temperature, thereby reducing the recovery rate of palladium, controlling the solution temperature to be less than 45 ℃, filtering, washing filter residues with hydrochloric acid with the pH value of 1, complexing ammonia water and acidifying hydrochloric acid for 3-4 times, finally obtaining pure dichlorodiamine palladium, slurrying pure dichlorodiamine palladium with water, heating to 40-50 ℃, slowly adding hydrazine hydrate, adding hydrazine hydrate to be not too fast, otherwise, generating palladium powder particles to be larger, easily bringing out impurity elements to influence the purity of palladium powder, drying palladium powder for 4h at 120 ℃ after washing with water, and obtaining the palladium sponge powder.
The reaction device used in the step S1 comprises a reaction kettle 1, wherein the inner side of the reaction kettle 1 is provided with a stirring mechanism, the bottom of the stirring mechanism is provided with an air outlet mechanism, the upper side of the reaction kettle 1 is provided with a feeding mechanism which is matched with the stirring mechanism and is used for intermittent feeding, both sides of the outer part of the reaction kettle 1 are provided with shaking mechanisms, the stirring mechanism comprises a transmission sleeve 2 which is rotationally 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, the output end of the driving motor 5 is fixedly connected with a driving gear 4, one side of the driving gear 4 is meshed with a driven gear 6 which is fixedly sleeved with the outer side of the transmission sleeve 2, the lower side of the transmission sleeve 2 is horizontally rotationally connected with a plurality of cross bars 34 which are positioned in the reaction kettle 1, the outer sides of the cross bars 34 are fixedly connected with a plurality of vertical bars 36 which are vertically arranged, the outer surfaces of the vertical bars 36 are fixedly connected with a plurality of crushing teeth 35, the second bevel gears 32 positioned at the inner side of the transmission sleeve 2 are fixedly sleeved at one ends of the cross rods 34, the fixed rods 18 fixedly connected with the bottom of the inner side of the reaction kettle 1 are movably arranged at the inner side of the transmission sleeve 2, the fixed rods 18 are fixedly sleeved with the first bevel gears 31 meshed with the second bevel gears 32, the inner sides of the cross 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 rods 18, the inner side of the fixed rods 18 is provided with an air inlet cavity communicated with the air outlet sleeve 29, the two ends of the inner side of the air outlet sleeve 29 are respectively fixedly connected with springs 28, one ends of the two springs 28 are respectively fixedly connected with a sliding block 27 which is in sliding connection 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 feed pipe 24 communicated with the upper side of the reaction kettle 1, the middle of the feed pipe 24 is connected with a limit sleeve 21, the inner side of the limit sleeve 21 is rotationally connected with a rotary gear 22, a discharging hole 23 matched with the feed 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, the center of the rotary gear 22 is fixedly sleeved with a stirring bracket 25 rotationally connected with the inner side of the raw material box 7, 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, and the discharging hole 23 on the rotary gear 22 is intermittently matched with the feed pipe 24, the platinum and palladium furnace powder in the raw material box 7 intermittently flows into the reaction kettle 1 to react with hydrochloric acid in batches, so that the reaction is more sufficient, the reaction rate is improved, the intermediate gear 20 rotates and drives the stirring bracket 25 to rotate in the raw material box 7, the platinum and palladium furnace powder can enter the feed pipe 24 more rapidly and then flow into the reaction kettle 1, the feed pipe 24 is prevented from being blocked by the platinum and palladium furnace powder, the feeding of the platinum and palladium furnace powder is influenced, the platinum, palladium furnace powder and hydrochloric acid can be stirred by 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 by the heating pipe 33 in the cross rod 34 and the vertical rod 36, the reaction temperature is initially controlled to be 80-85 ℃, and the platinum, the reaction rate of the palladium furnace powder and hydrochloric acid is fastest, meanwhile, the rapid increase of the temperature of the solution is facilitated, the subsequent purification time of platinum and palladium from the platinum and palladium furnace powder is reduced, when the platinum and palladium furnace powder is completely dissolved into hydrochloric acid, chlorine is pumped into the fixing rod 18 through the upper end of the fixing rod 18 through an air inlet cavity formed in the fixing rod 18, 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, the sliding block 27 opens the air outlet hole 30 on the upper side of the air outlet sleeve 29, then the chlorine enters the reaction kettle 1 through the air outlet hole 30, meanwhile, the temperature of the solution is increased to above 85 ℃ through the heating pipe 33, the platinum and palladium in the solution can be precipitated in the form of ammonium chloroplatinate and ammonium chloropalladate, and then the solution is cooled to room temperature.
The shaking mechanism comprises a plurality of supporting rods 13 movably arranged on the outer side of the reaction kettle 1, the upper ends of the supporting rods 13 are fixedly connected with a guide sleeve 11, the inner side of the guide sleeve 11 is slidably connected with an arc-shaped rack 12 fixedly connected with the side wall of the reaction kettle 1, the top end of the supporting rod 13 is fixedly connected with an adjusting motor 10, the output end of the adjusting motor 10 is fixedly connected with an adjusting gear 9 meshed with the arc-shaped rack 12, the adjusting gear 9 is driven to rotate through the adjusting motor 10, the arc-shaped rack 12 is further rotated, the reaction kettle 1 can swing left and right in a reciprocating manner, mixed liquid in the reaction kettle 1 is stirred more fully, and when sediment is discharged, the reaction kettle 1 can be rotated for a certain angle, so that a discharge opening is positioned at the lowest position, sediment inside the reaction kettle 1 is conveniently and rapidly discharged, and the discharge rate is improved.
The second scraping plates 19 which are movably arranged on the inner side wall of the reaction kettle 1 are fixedly connected to one ends of the cross rods 34, which are far away from the transmission sleeve 2, the connecting rods 16 which are obliquely arranged are fixedly connected to the lower ends of the transmission sleeve 2, the first scraping plates 17 which are slidably arranged on the bottom of the inner side of the reaction kettle 1 are fixedly connected to the lower ends of the connecting rods 16, the platinum and palladium furnace powder on the inner side wall and the bottom of the reaction kettle 1 can be scraped off through the first scraping plates 17 and the second scraping plates 19, the platinum and palladium furnace powder can be fully reacted with hydrochloric acid, the platinum and palladium furnace powder can be quickly dissolved in the hydrochloric acid, the purification recovery rate of subsequent platinum and palladium can be improved, and the use is convenient.
The upside of reation kettle 1 is provided with feed liquor pipe 3 and blast pipe 8, and the bottom of reation kettle 1 is provided with drain pipe 15, and the upper end of drain pipe 15 is provided with the filter screen, and discharge opening 26 has still been seted up to bottom one side of reation kettle 1, and the outside of reation kettle 1 is provided with the discharge gate 14 with discharge opening 26 complex, discharges liquid through drain pipe 15 for the precipitate passes through discharge opening 26 discharge, just can carry out subsequent purification process, further shortens the required time of purification.
Working principle: the platinum and palladium furnace powder is poured into the raw material tank 7, then hydrochloric acid is added into the reaction kettle 1 through the liquid inlet pipe 3, then the driving motor 5 drives the transmission sleeve 2 to rotate through the 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 on the rotary gear 22 is intermittently matched with the feeding pipe 24, further, the platinum and palladium furnace powder in the raw material tank 7 intermittently flows into the reaction kettle 1, the platinum and palladium furnace powder is reacted with the hydrochloric acid in batches, thus the reaction is more complete, the reaction rate is improved, the intermediate gear 20 rotates and simultaneously drives the stirring bracket 25 to rotate in the raw material tank 7, the platinum and palladium furnace powder can more rapidly enter the feeding pipe 24 and further flow 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 powder is influenced, the platinum and palladium furnace powder and 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 initially controlled to be 80-85 ℃, the reaction rate of the platinum and palladium furnace powder and the hydrochloric acid can be fastest, the temperature of the solution can be conveniently and rapidly improved, the time for purifying the platinum and palladium from the platinum and palladium furnace powder is reduced, when the platinum and palladium furnace powder is completely dissolved in the hydrochloric acid, the 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, flows into the air outlet sleeve 29, the spring 28 is compressed by the sliding block 27 on the inner side of the air outlet sleeve 29, the air outlet hole 30 on the upper side of the air outlet sleeve 29 is opened by the sliding block 27, chlorine enters the reaction kettle 1 through the air outlet hole 30, meanwhile, the temperature of the solution is raised to be higher than 85 ℃ by the heating pipe 33, platinum and palladium in the solution can be precipitated in the form of ammonium chloroplatinate and ammonium chloropalladate, then the solution is cooled to room temperature, then liquid is discharged through the liquid outlet pipe 15, sediment is discharged through the discharge opening 26, the subsequent purification process can be performed, the time required by purification is further shortened, the regulating gear 9 is driven to rotate by the regulating motor 10, the arc-shaped rack 12 is further driven to rotate, the reaction kettle 1 can swing in a left-right reciprocating manner, the mixed liquid in the reaction kettle 1 is more fully stirred, the reaction kettle 1 can be rotated by a certain angle when the sediment is discharged, the sediment in the reaction kettle 1 is discharged conveniently and rapidly, and the discharge rate is improved.
In the description of the present invention, it should 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", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. A refining and purifying process for platinum and palladium furnace powder 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, 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 4h until the solid is completely dissolved;
s2: then heating the solution to above 85 ℃, then introducing chlorine, controlling the potential of the chlorine to 390-410 mV in the reaction process, precipitating platinum and palladium in the form of ammonium chloroplatinate and ammonium chloropalladate, cooling to room temperature, filtering, washing the ammonium chloroplatinate and ammonium chloropalladate coprecipitate for 4-5 times by using 10% ammonium chloride saturated solution, and washing impurities;
s3: because the solubility of ammonium chloroplatinate and ammonium chloropalladate in water is different, adding water into the mixture of ammonium chloroplatinate and ammonium chloropalladate according to the liquid-solid ratio (3-4) of 1, boiling 2 h to completely dissolve the ammonium chloropalladate in the solution, filtering, purifying palladium from the filtrate and purifying platinum from the filter residue;
s4: refining of platinum
Taking filter residues treated in the step S3, slowly adding aqua regia according to the liquid-solid ratio (2-3), controlling the temperature at 85-90 ℃, reacting at 3-h, filtering after the reaction, removing nitric acid from filtrate, evaporating the filtrate to paste, adding concentrated hydrochloric acid, removing nitric acid for 2-3 times again, adding 1% of dilute hydrochloric acid to boil and dissolve, heating and boiling for a period of time, adding ammonium chloride until no yellow precipitate is generated, then rapidly cooling by circulating cooling water, cooling to room temperature, finally filtering, and filtering; washing filter residues 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 constant temperature at 2 h, heating to 400-450 ℃, keeping the constant temperature at 1-2 h, heating to 750 ℃, keeping the constant temperature at 2-3 h, and slowly cooling to obtain light gray sponge platinum;
s5: refining of palladium
And (3) heating the filtrate treated in the step (S3) to above 85 ℃, slowly adding an oxidant and ammonium chloride until no red precipitate is generated, filtering after the reaction is finished, washing filter residues with 10% ammonium chloride solution, adding water into ammonium chloropalladate, boiling 2 for h to completely dissolve the ammonium chloropalladate, cooling and filtering, continuously precipitating palladium from the filtrate, repeating the processes of ammonium chloride palladium precipitation and water dissolution for 1-2 times, effectively removing common metals in the process, finally obtaining pure ammonium chloropalladate, and then mixing the pure ammonium chloropalladate according to a liquid-solid ratio (3-4): 1, adding water for pulping, adding concentrated ammonia water to adjust the pH value to 8-9, heating to 80 ℃, adding ammonia water in the reaction process, maintaining the pH value of the solution to 8-9, reacting to 1-h, cooling and filtering, slowly adding hydrazine hydrate because dichlorotetra-ammine palladium and hydrochloric acid are exothermic reaction, slowly adding concentrated hydrochloric acid into the ammonia water complexing solution until the pH value is 1, otherwise, generating soluble cis-dichlorodi-ammine palladium by excessively high solution temperature, thereby reducing the recovery rate of palladium, controlling the solution temperature to be less than 45 ℃, filtering, washing filter residues with hydrochloric acid with the pH value of 1, complexing ammonia water and acidifying hydrochloric acid for 3-4 times, finally obtaining pure dichlorodiamine palladium, slurrying pure dichlorodiamine palladium with water, heating to 40-50 ℃, slowly adding hydrazine hydrate, adding hydrazine hydrate to be not too fast, otherwise, generating palladium powder particles to be larger, easily bringing out impurity elements to influence the purity of palladium powder, drying palladium powder for 4h at 120 ℃ after washing with water, and obtaining the palladium sponge powder.
2. The refining and purifying process of platinum and palladium furnace powder according to claim 1, wherein the reaction device used in the step S1 comprises a reaction kettle (1), 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 for intermittent feeding matched with the stirring mechanism is arranged on the upper side of the reaction kettle (1), and shaking mechanisms are arranged on two sides of the outer part of the reaction kettle (1).
3. The refining and purifying process for platinum and palladium furnace powder according to claim 2, wherein the stirring mechanism comprises a transmission sleeve (2) which is rotationally connected with the inner side of the reaction kettle (1) in the vertical direction, a driving motor (5) is fixedly connected to the upper side of the reaction kettle (1), a driving gear (4) is fixedly connected to the output end of the driving motor (5), a driven gear (6) fixedly sleeved on the outer side of the transmission sleeve (2) is meshed with one side of the driving gear (4), a plurality of cross rods (34) which are positioned in the reaction kettle (1) are horizontally rotationally connected to the lower side of the transmission sleeve (2), a plurality of vertical rods (36) which are vertically arranged are fixedly connected to the outer side of the cross rods (34), a plurality of crushing teeth (35) are fixedly sleeved on one end of each cross rod (34), a second bevel gear (32) which is positioned on the inner side of the transmission sleeve (2), a fixing rod (18) fixedly sleeved on the inner side bottom of the reaction kettle (1) is movably arranged, and a plurality of heating pipes (33) are fixedly sleeved on one end of the fixing rods (18), and each fixing rod (33) is fixedly sleeved on one end of each heating pipe (33).
4. The refining and purifying process of platinum and palladium furnace powder according to claim 3, wherein the air outlet mechanism comprises an air outlet sleeve (29) fixedly connected with the lower end of a fixed rod (18), an air inlet cavity communicated with the air outlet sleeve (29) is formed in the inner side of the fixed rod (18), springs (28) are fixedly connected to the two ends of the inner side of the air outlet sleeve (29), sliding blocks (27) connected with the inner side of the air outlet sleeve (29) in a sliding mode are fixedly connected to one ends of the springs (28), and air outlet holes (30) matched with the sliding blocks (27) are formed in the upper side of the air outlet sleeve (29).
5. The refining and purifying process for platinum and palladium furnace powder 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), a feeding pipe (24) communicated with the upper side of the reaction kettle (1) is communicated with the lower end of the raw material box (7), a limiting sleeve (21) is connected in the middle of the feeding pipe (24), a rotary gear (22) is rotatably connected with the inner side of the limiting sleeve (21), a blanking hole (23) matched with the feeding pipe (24) is formed in the rotary gear (22), an intermediate gear (20) meshed with a driven gear (6) is meshed with one side of the rotary gear (22), and a stirring bracket (25) rotatably connected with the inner side of the raw material box (7) is fixedly sleeved at the center of the rotary gear (22).
6. The refining and purifying process of platinum and palladium furnace powder according to claim 2, wherein the shaking mechanism comprises a plurality of support rods (13) movably arranged on the outer side of the reaction kettle (1), the upper ends of the support rods (13) are fixedly connected with guide sleeves (11), the inner sides of the guide sleeves (11) are slidably connected with arc 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 racks (12).
7. The refining and purifying process for platinum and palladium furnace powder according to claim 3, wherein one ends of the cross rods (34) far away from the transmission sleeve (2) are fixedly connected with second scrapers (19) movably arranged on the inner side wall of the reaction kettle (1), the lower ends of the transmission sleeve (2) are fixedly connected with a plurality of connecting rods (16) obliquely arranged, and the lower ends of the connecting rods (16) are fixedly connected with first scrapers (17) slidably arranged on the bottom of the inner side of the reaction kettle (1).
8. The refining and purifying process of platinum and palladium furnace powder according to claim 2, wherein 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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| 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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| 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 |
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