CN112322900B - Method for extracting platinum, palladium and rhodium from automobile exhaust waste catalyst - Google Patents
Method for extracting platinum, palladium and rhodium from automobile exhaust waste catalyst Download PDFInfo
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- CN112322900B CN112322900B CN202011188780.9A CN202011188780A CN112322900B CN 112322900 B CN112322900 B CN 112322900B CN 202011188780 A CN202011188780 A CN 202011188780A CN 112322900 B CN112322900 B CN 112322900B
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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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- C22B1/02—Roasting processes
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- 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 discloses a method for extracting platinum, palladium and rhodium from a waste catalyst of automobile exhaust, which comprises the following steps: (1) Crushing the automobile exhaust waste catalyst and then roasting to obtain roasting slag; (2) Mechanically activating the roasting slag by using ball milling equipment to obtain an activated material; (3) Leaching the activating material, wherein stannous chloride is used as a leaching agent in the leaching solution, and the leaching agent is dissolved in a dilute hydrochloric acid solution to form the activating material; the leaching process conditions are as follows: the solid-liquid ratio of the activating material to the leaching solution is (2-5): 1. the concentration of the dilute hydrochloric acid solution is 0.5-5 mol/L, the concentration of stannous chloride is 0.05-1.0 mol/L, the leaching reaction temperature is 30-100 ℃, and the leaching reaction time is 30-120 min. The invention adopts stannous chloride as the leaching agent and does not generate any harmful gas; can effectively avoid the corrosion of high-acid and high-corrosivity environment to equipment.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of resources, and particularly relates to a method for extracting platinum, palladium and rhodium from a waste catalyst of automobile exhaust.
Background
The recovery method of the platinum, palladium and rhodium of the waste catalyst of the automobile exhaust comprises two major methods, namely a pyrogenic method and a wet method. The advantages of the pyrometallurgical recovery process include large treatment capacity, strong material adaptability and stable recovery rate, but also have the defects of high energy consumption, large equipment investment, large slag quantity and the like. The wet recovery process has the advantages of less equipment investment, flexible treatment capacity, short process and the like, but has the defect of unstable recovery rate. The existing wet recovery process usually comprises three parts of pretreatment, wet crude extraction and refining, and because the oxidation state of the platinum, the palladium and the rhodium is difficult to recover by a common water-chlorine method, the existing wet process converts the oxidation state and the wrapped platinum group metal in the waste catalyst into a simple substance state by combining pretreatment means such as oxidizing roasting, ball milling, reducing leaching and the like, so that the subsequent leaching by the water-chlorine method is convenient, however, the fluctuation range of the comprehensive leaching rate of the wet process is large due to the influence of materials and process conditions, the residual grade of the platinum, the palladium and the rhodium in the leaching residue is still 100-150 g/t, and the economy of the wet process is greatly reduced.
Disclosure of Invention
Aiming at the defects of the existing fire method and wet method processes, the invention provides an environment-friendly and efficient method for recovering platinum, palladium and rhodium in the automobile exhaust waste catalyst by using a full-oxidation roasting-high-energy ball-milling activation-acidic stannous chloride leaching method, and the problems of long process, environmental pollution and the like existing in the existing process are solved.
The invention adopts the following technical scheme:
a method for extracting platinum, palladium and rhodium in a waste catalyst of automobile exhaust is characterized by comprising the following steps:
(1) Crushing the automobile exhaust waste catalyst and then roasting to obtain roasting slag; the roasting process conditions are as follows: the roasting temperature is 500-900 ℃, and the roasting time is 1-3 h;
(2) Mechanically activating the roasting slag by using ball milling equipment to obtain an activated material; the process conditions for mechanical activation of the roasting slag by adopting ball milling equipment are as follows: the ball material ratio is (5-15): 1. the rotating speed is 400 to 800 revolutions per minute, and the ball milling time is 15 to 60min;
(3) Leaching the activating material, wherein the leaching solution for leaching the activating material is formed by taking stannous chloride as a leaching agent and dissolving the leaching agent in a dilute hydrochloric acid solution; the leaching process conditions are as follows: the solid-liquid ratio of the activating material to the leaching solution is (2-5): 1. the concentration of the dilute hydrochloric acid solution is 0.5-5 mol/L, the concentration of stannous chloride is 0.05-1.0 mol/L, the leaching reaction temperature is 30-100 ℃, and the leaching reaction time is 30-120 min.
The method for extracting platinum, palladium and rhodium from the waste automobile exhaust catalyst is characterized in that the granularity of the crushed waste automobile exhaust catalyst in the step (1) is as follows: the content of more than 400 meshes is 0 to 20 percent, and the content of less than 400 meshes is 80 to 100 percent.
The method for extracting the platinum, the palladium and the rhodium in the automobile exhaust waste catalyst is characterized in that in the step (1), the roasted material is stirred every 15-30 min in the roasting process after the automobile exhaust waste catalyst is crushed.
The invention has the beneficial technical effects that: according to the method, the platinum, palladium and rhodium in the waste catalyst are converted into an oxidation state by a roasting mode, the platinum, palladium and rhodium in the waste catalyst are extracted by an acidic stannous chloride method instead of a water-chlorine method which is most commonly used in the traditional wet process, so that stannous chloride is used as a leaching agent without generating any harmful gas, the problem of chlorine pollution generated by the water-chlorine method can be solved, the hydrochloric acid concentration of a stannous chloride method system is only 1-5 mol/L and is far lower than the acid concentration in the water-chlorine method, and therefore the corrosion of high-acid and high-corrosivity environment to equipment can be effectively avoided.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Referring to fig. 1, the method for extracting platinum, palladium and rhodium from the waste catalyst of automobile exhaust comprises the following steps:
(1) And (3) full-oxidation roasting: and fully crushing the automobile exhaust waste catalyst, and then placing the crushed automobile exhaust waste catalyst in a muffle furnace for roasting to obtain roasted slag. The waste catalyst for automobile exhaust comprises platinum, palladium, rhodium and Al 2 O 3 、SiO 2 、MgO、CeO 2 、ZrO 2 、La 2 O 3 Wherein the content of platinum is 100-850 g/t, the content of palladium is 500-1627 g/t, the content of rhodium is 20-320 g/t, siO 2 18.12-35.23 percent of magnesium oxide (MgO), 4.65-10.12 percent of CeO 2 The mass percentage content of the ZrO 2.77-3.54 percent 2 2.50-9.81% of La 2 O 3 The mass percentage content of the alloy is 3.66-6.65 percent, and the rest is Al 2 O 3 . The granularity of the crushed automobile exhaust waste catalyst is as follows: the content of more than 400 meshes is 0 to 20 percent, and the content of less than 400 meshes is 80 to 100 percent. The crushed powder is roasted in a muffle furnace under the air atmosphere, the roasting can fully oxidize coke loaded on the surface of the platinum, the palladium and the rhodium in the automobile exhaust waste catalyst, so that the platinum, the palladium and the rhodium are fully oxidized, and alpha-Al in a coating is prevented 2 O 3 Conversion to sparingly soluble gamma-Al 2 O 3 Wrapping platinum, palladium and rhodium, controlling the roasting temperature to be 500-900 ℃ and the roasting time to be 1-3 h; stirring the roasting material once every 15-30 min in the roasting process to fully oxidize the platinum, the palladium, the rhodium and organic matters in the roasting slag, fully contacting the platinum, the palladium and the rhodium by oxygen and converting the platinum, the palladium and the rhodium in a simple substance state into PtO in an oxide state 2 、PdO、Rh 2 O 3 . The roasting material is the crushed automobile exhaust waste catalyst.
(2) High-energy ball milling: the roasting slag is mechanically activated by high-energy planetary ball milling equipment, and the purpose of activation is to fully expose platinum, palladium and rhodium in the waste catalyst, facilitate the contact with a leaching reagent, fully refine lump materials formed by sintering due to local overheating, prevent the sintering lump from forming secondary package on the platinum, the palladium and the rhodium, and enable the PtO 2 、PdO、Rh 2 O 3 Fully dissociative and expose. Obtaining an activated material after mechanical activation; the process conditions for mechanical activation of the roasting slag by adopting ball milling equipment are as follows: the ball material ratio is (5-15): 1. the rotating speed is 400 to 800 revolutions per minute, and the ball milling time is 15 to 60min.
(3) Leaching by a stannous chloride method: leaching the activating material in the leaching solution, wherein the leaching solution is formed by taking stannous chloride as a leaching agent and dissolving the leaching agent in a dilute hydrochloric acid solution; complexation of stannous chloride to PtO 2 、PdO、Rh 2 O 3 Conversion to the corresponding complex ion [ PtCl ] 3 (SnCl 3 )] 2- 、[PdCl 3 (SnCl 3 )] 2- 、[RhCl 2 (SnCl 3 )] 2- . The leaching process conditions are as follows: the mass ratio of the activating material to the leaching solution is (2-5): 1. the concentration of the dilute hydrochloric acid is 0.5-5 mol/L, the concentration of the stannous chloride is 0.05-1.0 mol/L, the leaching reaction temperature is 30-100 ℃, and the leaching reaction time is 30-120 min.
The chemical reaction equation related to the invention is as follows:
C+O 2 ＝CO 2
Pt+O 2 ＝PtO 2
2Pd+O 2 ＝2PdO
4Rh+3O 2 ＝2Rh 2 O 3
PtO 2 +2SnCl 2 +4H + +6Cl - ＝[PtCl 3 (SnCl 3 )] 2- +2H 2 O+SnCl 4
PdO+SnCl 2 +2H + +4Cl - ＝[PdCl 3 (SnCl 3 )] 2- +H 2 O
Rh 2 O 3 +4SnCl 2 +6H + +10Cl - ＝2[RhCl 2 (SnCl 3 )] 2- +3H 2 O+2SnCl 4
example 1
The content of platinum in the automobile exhaust waste catalyst is 850g/t, the content of palladium is 1627g/t, the content of rhodium is 320g/t, and Al 2 O 3 33.21 percent of SiO 2 35.23 percent of magnesium oxide, 4.65 percent of MgO and CeO 2 Is 3.54 percent of ZrO 2 The mass percentage of the La is 2.50 percent 2 O 3 The mass percentage of (B) is 3.66%.
Fully crushing 2kg of the automobile exhaust waste catalyst, wherein the crushed granularity is as follows: the content of more than 400 meshes is 5 percent, and the content of less than 400 meshes is 95 percent. Placing the crushed automobile exhaust waste catalyst into an iron boat, and placing the iron boat into a muffle furnace to be roasted under an air atmosphere to obtain roasted slag; the roasting temperature is 750 ℃, the roasting time is 1h, and the roasted material is stirred every 15min in the roasting process, so that oxygen fully contacts the platinum, palladium and rhodium.
Placing the roasting slag in a high-energy planetary ball mill for mechanical activation to obtain an activated material; the mechanical activation process conditions of the roasting slag by adopting the high-energy planetary ball mill are as follows: the ball material ratio is 8: 1. the rotating speed is 600 r/min, and the ball milling time is 15min.
The activating material is leached from the leaching solution, stannous chloride is used as a leaching agent in the leaching solution, and the leaching agent is dissolved in dilute hydrochloric acid solution to form the activating material. The leaching process conditions are as follows: the mass ratio of the activating material to the leaching solution is 4: 1. the concentration of the dilute hydrochloric acid solution is 1.5mol/L, the concentration of stannous chloride is 0.05mol/L, the leaching reaction temperature is 40 ℃, and the leaching reaction time is 60min. After the leaching reaction is finished, carrying out solid-liquid separation by using a suction filtration device, and washing twice by using dilute hydrochloric acid.
After being dried, the leaching residue obtained by the treatment process is subjected to fire test gold enrichment-aqua regia digestion, and the leaching rates of platinum, palladium and rhodium in the leaching residue are respectively 99%, 99% and 95%.
Example 2
The content of platinum, palladium and rhodium in the automobile exhaust waste catalyst is 100g/t, 500g/t and 20g/t respectively, and Al 2 O 3 Is 30 percent by mass and SiO 2 35.23 percent of magnesium oxide, 10.12 percent of MgO and CeO 2 Is 3.54 percent by mass, zrO 2 Is 2.50 percent of La 2 O 3 The content of (b) is 3.66% by mass.
Fully crushing 2kg of the automobile exhaust waste catalyst, wherein the crushed granularity is as follows: the content of more than 400 meshes is 10 percent, and the content of less than 400 meshes is 90 percent. Placing the crushed automobile exhaust waste catalyst into an iron boat, and placing the iron boat into a muffle furnace to be roasted under an air atmosphere to obtain roasted slag; the roasting temperature is 500 ℃, the roasting time is 3 hours, and the roasted material is stirred every 20min in the roasting process, so that oxygen is fully contacted with the platinum, palladium and rhodium.
Placing the roasting slag in a high-energy planetary ball mill for mechanical activation to obtain an activated material; the process conditions for mechanically activating the roasting slag by adopting the high-energy planetary ball mill are as follows: the ball material ratio is 5: 1. the rotating speed is 400 r/m, and the ball milling time is 40min.
Leaching the activating material in the leaching liquid, wherein the leaching liquid takes stannous chloride as a leaching agent, and the leaching agent is dissolved in a dilute hydrochloric acid solution to form the activated material. The leaching process conditions are as follows: the mass ratio of the activating material to the leaching solution is 2: 1. the concentration of the dilute hydrochloric acid solution is 5mol/L, the concentration of stannous chloride is 0.5mol/L, the leaching reaction temperature is 70 ℃, and the leaching reaction time is 120min. After the leaching reaction is finished, carrying out solid-liquid separation by using a suction filtration device, and washing twice by using dilute hydrochloric acid.
After being dried, the leaching residue obtained by the treatment process is subjected to fire test gold enrichment and aqua regia digestion, and the leaching rates of platinum, palladium and rhodium in the leaching residue are respectively 99 percent, 99 percent and 98 percent.
Example 3
The content of platinum in the automobile exhaust waste catalyst is 500g/t, the content of palladium is 100g/t, the content of rhodium is 200g/t, and Al is 2 O 3 Is 25.11 percent of SiO 2 25.01 percent by mass, 7.12 percent by mass of MgO and CeO 2 Is 4.54 percent by mass, zrO 2 The mass percentage of the La is 7.50 percent 2 O 3 The mass percentage of (B) is 4.66%.
Fully crushing 2kg of the automobile exhaust waste catalyst, wherein the crushed granularity is as follows: the content of more than 400 meshes is 20 percent, and the content of less than 400 meshes is 90 percent. Placing the crushed automobile exhaust waste catalyst into an iron boat, and placing the iron boat into a muffle furnace to be roasted under an air atmosphere to obtain roasted slag; the roasting temperature is 900 ℃, the roasting time is 2h, and the roasted material is stirred every 30min in the roasting process, so that oxygen fully contacts the platinum, palladium and rhodium.
Placing the roasting slag in a high-energy planetary ball mill for mechanical activation to obtain an activated material; the mechanical activation process conditions of the roasting slag by adopting the high-energy planetary ball mill are as follows: the ball material ratio is 15: 1. the rotating speed is 800 r/m, and the ball milling time is 60min.
Leaching the activating material in the leaching liquid, wherein the leaching liquid takes stannous chloride as a leaching agent, and the leaching agent is dissolved in a dilute hydrochloric acid solution to form the activated material. The leaching process conditions are as follows: the solid-to-liquid ratio of the activating material to the leaching solution is 5: 1. the concentration of the dilute hydrochloric acid solution is 3mol/L, the concentration of stannous chloride is 1.0mol/L, the leaching reaction temperature is 50 ℃, and the leaching reaction time is 30min. After the leaching reaction is finished, carrying out solid-liquid separation by using a suction filtration device, and washing twice by using dilute hydrochloric acid.
After being dried, the leaching residue obtained by the treatment process is subjected to fire test gold enrichment-aqua regia digestion, and the leaching rates of platinum, palladium and rhodium in the leaching residue are respectively 99%, 99% and 98%.
Claims (2)
1. A method for extracting platinum, palladium and rhodium from an automobile exhaust waste catalyst is characterized by comprising the following steps:
(1) Crushing the automobile exhaust waste catalyst and then roasting to obtain roasting slag; the roasting process conditions are as follows: the roasting temperature is 500-900 ℃, and the roasting time is 1-3 h; the waste catalyst for automobile exhaust comprises platinum, palladium, rhodium and Al 2 O 3 、SiO 2 、MgO、CeO 2 、ZrO 2 、La 2 O 3 Wherein the content of platinum is 100-850 g/t, the content of palladium is 500-1627 g/t, the content of rhodium is 20-320 g/t, and SiO 2 18.12-35.23 percent of magnesium oxide (MgO), 4.65-10.12 percent of CeO 2 The mass percentage of the ZrO 2.77-3.54 percent 2 The mass percentage of the La is 2.50-9.81 percent 2 O 3 The mass percentage of the Al-based alloy is 3.66-6.65 percent, and the balance is Al 2 O 3 (ii) a The granularity of the crushed automobile exhaust waste catalyst is as follows: the content of more than 400 meshes is 0 to 20 percent, and the content of less than 400 meshes is 80 to 100 percent;
(2) Mechanically activating the roasting slag by using ball milling equipment to obtain an activated material; the process conditions for mechanical activation of the roasting slag by adopting ball milling equipment are as follows: the ball material ratio is (5-15): 1. the rotating speed is 400 to 800 revolutions per minute, and the ball milling time is 15 to 60min;
(3) Leaching the activating material, wherein the leachate for leaching the activating material is formed by taking stannous chloride as a leaching agent and dissolving the leaching agent in a dilute hydrochloric acid solution; the leaching process conditions are as follows: the solid-liquid ratio of the activating material to the leaching solution is (2-5): 1. the concentration of the dilute hydrochloric acid solution is 0.5-5 mol/L, the concentration of stannous chloride is 0.05-1.0 mol/L, the leaching reaction temperature is 30-100 ℃, and the leaching reaction time is 30-120 min.
2. The method for extracting platinum, palladium and rhodium from the waste automobile exhaust catalyst according to claim 1, wherein in the step (1), the roasted material is stirred every 15min to 30min in the roasting process after the waste automobile exhaust catalyst is crushed.
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| CN108265180A (en) * | 2017-12-28 | 2018-07-10 | 核工业北京化工冶金研究院 | The leaching method of platinum, palladium, rhodium in useless three-way catalyst |
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