CN110684905A - Method for leaching metal platinum in platinum alumina catalyst by wet method - Google Patents
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- 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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Abstract
The invention discloses a method for leaching metal platinum in a platinum alumina catalyst by a wet method, which comprises the following steps: (1) filling a platinum alumina catalyst into a reaction tube of a fixed bed reactor, and replacing air in the reaction tube with nitrogen; (2) introducing reducing gas, heating to activate the platinum alumina catalyst, and naturally cooling to room temperature; (3) introducing water from the bottom of the reaction tube, wetting the platinum alumina catalyst, heating by microwave to 60-90 ℃, keeping the temperature, keeping the catalyst fixed, and introducing hydrogen chloride gas and sodium percarbonate solution from the bottom of the reaction tube for reaction; (4) and the residual solid in the reaction tube is recycled after being washed and dried. The method provided by the invention has the advantages that the recovery rate of platinum can reach more than 98%, the alumina carrier is not damaged in the leaching process, and the carrier can be used as the raw material for producing the catalyst again.
Description
Technical Field
The invention belongs to the technical field of precious metal catalyst recovery, and particularly relates to a method for leaching metal platinum in a platinum alumina catalyst by a wet method.
Background
The waste platinum alumina catalyst contains nano-grade noble metal platinum and can be recycled. In the traditional technology, aqua regia is used for dissolving the catalyst, but the method has large discharge amount of nitrogen oxides and serious damage degree to the alumina carrier, and platinum ions dissolved by the aqua regia are easy to be adsorbed on the alumina carrier again, so the dissolving efficiency is low, and the content of platinum on the carrier can be gradually reduced only by continuously replenishing fresh aqua regia, so the using amount of the aqua regia is large. The aqua regia dissolves much aluminum oxide, forms a large amount of aluminum chloride and aluminum nitrate in the solution, and is easy to hydrolyze due to overhigh aluminum concentration to form aluminum sol, so that the subsequent filtering operation can not be basically realized. In addition, the formed aluminum sol may contain a certain amount of platinum ions, and the platinum ions cannot enter into the filtrate during filtration, so that platinum loss is caused, and the recovery rate is low. Chinese patent 201711463718.4 discloses a method for recovering platinum from an aluminum-based catalyst by using a soluble carrier, which comprises selectively dissolving alumina in a waste platinum alumina catalyst, reducing the solution to make the noble metal platinum solid, filtering and separating the crude platinum, and refining and purifying the crude platinum. Alumina belongs to inert materials, a large amount of acid is consumed for dissolving alumina, greater pollution exists, the solubility of alumina is poor, the volume of liquid after complete dissolution is large, aluminum ions are easy to hydrolyze into aluminum hydroxide and are difficult to filter, in addition, the platinum particles after reduction are small, the filtering difficulty is increased, the nano-scale platinum particles are hardly captured through a filter screen or a filter paper, the recovery rate of platinum is not high, and the analysis reason is that partial nano-scale platinum particles still exist in the filtrate and are difficult to capture and enrich. Chinese patent 201810979537.5 discloses a process for recovering platinum-rhenium-aluminium from waste platinum-rhenium catalyst with aluminium carrier, which also adopts a large amount of sulphuric acid to dissolve the whole aluminium carrier, then adopts ion exchange resin to enrich platinum-rhenium in the solution, and finally carries out purification and refining. The loss of platinum in the process may be in the filtering step, because the acid amount needed for completely dissolving the alumina is large, the volume after dissolving is also large, although the platinum in the solution is reduced or complexed into solid, because the particles are small, the filtering and washing are difficult, the hydrolysis of the aluminum is added to form aluminum hydroxide, and part of the platinum nano particles are wrapped in the aluminum hydroxide and are difficult to enrich, thereby causing certain influence on the recovery rate. Therefore, it is important to provide a method for recovering platinum metal from a platinum alumina catalyst.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for leaching metal platinum in a platinum alumina catalyst by a wet method, which has the advantages of small damage to an alumina carrier and high recovery rate of the metal platinum.
A method for leaching metal platinum in a platinum alumina catalyst by a wet method comprises the following steps:
(1) filling the platinum alumina catalyst into a reaction tube of a fixed bed reactor, and then replacing air in the reaction tube with nitrogen;
(2) introducing reducing gas, heating to the temperature of 300-600 ℃, activating the platinum alumina catalyst for 3-6h, and naturally cooling to the room temperature; the reducing gas is hydrogen chloride gas and hydrogen mixed with pyridine steam;
(3) introducing water from the bottom of the reaction tube, wetting the platinum alumina catalyst, heating by microwave to 60-90 ℃, continuously maintaining the temperature, keeping the catalyst fixed, introducing hydrogen chloride gas and 10-20wt% of sodium percarbonate solution from the bottom of the reaction tube, and reacting for 2-5 h;
(4) discharging the reacted gas at the top of the reaction tube, condensing and refluxing the gas into the reaction tube, and discharging the uncondensed gas after removing hydrogen chloride by alkali washing; leaching metal platinum ions in the reacted liquid, discharging the reacted liquid from the top of the reaction tube, and collecting the liquid for later use; and the residual solid in the reaction tube is recycled after being washed and dried, so that the alumina carrier is obtained.
Preferably, the platinum alumina catalyst is a platinum alumina catalyst for dehydrogenation of recovered alkane having a platinum content of 0.1 to 0.5wt%, or a platinum reforming catalyst having a platinum content of 0.1 to 0.5wt%, or a platinum alumina catalyst having a platinum content of 1 to 10 wt%.
Preferably, the hydrogen gas is mixed with 50-150ppm pyridine steam, and the volume ratio of the hydrogen chloride gas to the hydrogen gas mixed with the pyridine steam is 1: (600-800).
Preferably, the rate of temperature rise in step (2) is 1-3 ℃/min.
Preferably, the volume ratio of the hydrogen chloride gas to the sodium percarbonate solution in the step (3) is (100-) -200: 1, the volume ratio of the sodium percarbonate solution to the platinum alumina catalyst is (3-6.5): 1.
preferably, the rate of the microwave heating temperature rise is 0.5-1 ℃/min.
Preferably, the power of the microwave heating is 500-650W.
Preferably, the volume ratio of the flow rate of the nitrogen to the platinum alumina is (0.2-0.3L/min): 1L of the compound.
Preferably, the reaction tube in the step (1) is a quartz glass reaction tube.
Preferably, the fixed bed reactor in the step (1) is an overflow bed reactor, and the elution mode adopted is plug flow.
The invention has the advantages that:
1. the characteristics of an overflow bed (fixed bed) reactor are utilized, a plug flow elution mode is adopted, back mixing does not exist, eluted platinum ions cannot be adsorbed on an alumina carrier again, the leaching efficiency is high, the process is safe and environment-friendly, the three wastes are less, the recovery rate is high, and the recovery rate of platinum can reach more than 98%;
2. the platinum alumina catalyst is activated by introducing reducing gas, so that zero-valent metal platinum nanoparticles are favorably formed under the condition of high-temperature hydrogen, a large amount of chlorine and hydrogen are adsorbed on the platinum nanoparticles, the activated state is maintained, and the subsequent leaching is favorably realized;
3. the microwave heating is beneficial to the dissolution and leaching of platinum; the hydrogen chloride has certain solubility in water, the hydrogen chloride dissolved in the water forms hydrochloric acid to provide chloride ions for dissolving the nano platinum particles, and the undissolved hydrogen chloride gas plays a role in bubbling, so that the mass transfer effect of the system is enhanced, the liquid and gas are distributed more uniformly, and the effect of dissolving the platinum nano particles is enhanced; sodium percarbonate is decomposed in situ under reaction conditions to generate hydrogen peroxide and sodium carbonate, the hydrogen peroxide generated in situ provides an oxidant for dissolving the platinum nanoparticles, and the sodium carbonate can stabilize the acidity of the reaction and prevent alumina from being dissolved by strong acid;
4. the acidity of the system is weak, the condition is mild, the temperature is low, pyridine has a certain protection effect on alumina, the alumina carrier is not damaged in the leaching process, the carrier can be used as a raw material for producing the catalyst again, and the content of platinum remaining on the carrier is less than one ten thousandth;
5. nitric acid is not used, and nitrogen oxide emission is avoided; chlorine is not used, and the recovery process is safe; does not use concentrated hydrochloric acid and has low corrosiveness.
Detailed Description
Example 1
The adopted platinum alumina catalyst is a platinum alumina catalyst with platinum content of 0.3wt% for dehydrogenation of recovered alkane, wherein the physical parameters of an alumina carrier before being prepared into the platinum alumina catalyst are as follows: the specific surface area is 86.5m2The pore volume is 0.712mL/g, the pore diameter is 35.4nm, and the crushing strength is 35.5N; a platinum alumina catalyst having a platinum content of 0.3 wt.% and a specific surface area of 85.9m was prepared2The pore volume is 0.705mL/g, the pore diameter is 34.9nm, and the crushing strength is 35.2N;
a method for wet leaching metallic platinum from the platinum alumina catalyst, comprising the steps of:
(1) filling the platinum alumina catalyst into a reaction tube of an overflow bed reactor, and then replacing air in the reaction tube with nitrogen, wherein the volume ratio of the flow rate of the nitrogen to the volume of the platinum alumina is 0.2L/min: 1L; the reaction tube is a quartz glass reaction tube, the overflow bed reactor is one of fixed bed reactors, and the adopted elution mode is plug flow;
(2) introducing reducing gas, heating to 400 ℃ at the speed of 2 ℃/min to activate the platinum alumina catalyst for 5h, and naturally cooling to room temperature; the volume ratio of the reducing gas is 1: 700 parts by weight of hydrogen chloride gas and hydrogen gas mixed with pyridine vapor, the hydrogen gas being mixed with 100ppm of pyridine vapor;
(3) introducing water from the bottom of the reaction tube, wetting the platinum alumina catalyst, heating by microwave under 600W, heating to 80 ℃ at the speed of 1 ℃/min, keeping the catalyst fixed, introducing hydrogen chloride gas and 15wt% of sodium percarbonate solution from the bottom of the reaction tube, and reacting for 3 hours; the volume ratio of the hydrogen chloride gas to the sodium percarbonate solution is 150: 1, the volume ratio of the sodium percarbonate solution to the platinum alumina catalyst is 5: 1;
(4) discharging the reacted gas at the top of the reaction tube, condensing and refluxing the gas into the reaction tube, and discharging the uncondensed gas after removing hydrogen chloride by alkali washing; leaching metal platinum ions in the reacted liquid, discharging the reacted liquid from the top of the reaction tube, and collecting the liquid for later use; and the residual solid in the reaction tube is recycled after being washed and dried, so that the alumina carrier is obtained.
The content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier are detected, and the results are shown in table 1;
TABLE 1 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Wherein, the platinum recovery rate (%) = 1-platinum content in the recovered solid alumina support/platinum content in the platinum alumina catalyst;
as can be seen from Table 1, after the platinum-alumina catalyst is prepared by the alumina carrier and the platinum is leached by the wet method, the physical parameters of the alumina are not obviously changed, and the changes of the specific surface area, the pore volume and the pore diameter are small; the method has high recovery rate of the metal platinum and hardly damages an alumina carrier.
Example 2
The platinum alumina catalyst used is the platinum alumina catalyst with platinum content of 0.1wt% for the dehydrogenation of recovered alkane, wherein, the physical parameters of the alumina carrier are the same as the example 1, the platinum alumina catalyst with platinum content of 0.1wt% is prepared, and the specific surface area is 86.3m2The pore volume is 0.711mL/g, the pore diameter is 35.2nm, and the crushing strength is 35.3N;
a method for wet leaching metallic platinum from the platinum alumina catalyst, comprising the steps of:
(1) filling the platinum alumina catalyst into a reaction tube of an overflow bed reactor, and then replacing air in the reaction tube with nitrogen, wherein the volume ratio of the flow rate of the nitrogen to the volume of the platinum alumina is 0.2L/min: 1L; the reaction tube is a quartz glass reaction tube, the overflow bed reactor is one of fixed bed reactors, and the adopted elution mode is plug flow;
(2) introducing reducing gas, heating to 300 ℃ at the speed of 1 ℃/min to activate the platinum alumina catalyst for 6h, and naturally cooling to room temperature; the volume ratio of the reducing gas is 1: 600 parts per million (ppm) hydrogen chloride gas and hydrogen gas mixed with pyridine vapor, the hydrogen gas being mixed with 50ppm pyridine vapor;
(3) introducing water from the bottom of the reaction tube, wetting the platinum alumina catalyst, heating by microwave under the power of 500W, raising the temperature to 60 ℃ at the speed of 0.5 ℃/min, continuously keeping the temperature, keeping the catalyst fixed, introducing hydrogen chloride gas and 10wt% of sodium percarbonate solution from the bottom of the reaction tube, and reacting for 5 hours; the volume ratio of the hydrogen chloride gas to the sodium percarbonate solution is 100: 1, the volume ratio of the sodium percarbonate solution to the platinum alumina catalyst is 3: 1;
(4) discharging the reacted gas at the top of the reaction tube, condensing and refluxing the gas into the reaction tube, and discharging the uncondensed gas after removing hydrogen chloride by alkali washing; leaching metal platinum ions in the reacted liquid, discharging the reacted liquid from the top of the reaction tube, and collecting the liquid for later use; the residual solid in the reaction tube is recycled after being washed and dried;
the content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier are detected, and the results are shown in table 2;
TABLE 2 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Example 3
The platinum alumina catalyst used is the platinum alumina catalyst with platinum content of 0.5wt% for the dehydrogenation of recovered alkane, wherein, the physical parameters of the alumina carrier are the same as the example 1, the platinum alumina catalyst with platinum content of 0.5wt% is prepared, and the specific surface area is 85.7m2The pore volume is 0.706mL/g, the pore diameter is 34.6nm, and the crushing strength is 35.7N;
a method for wet leaching metallic platinum from the platinum alumina catalyst, comprising the steps of:
(1) filling the platinum alumina catalyst into a reaction tube of an overflow bed reactor, and then replacing air in the reaction tube with nitrogen, wherein the volume ratio of the flow rate of the nitrogen to the volume of the platinum alumina is 0.3L/min: 1L; the reaction tube is a quartz glass reaction tube, the overflow bed reactor is one of fixed bed reactors, and the adopted elution mode is plug flow;
(2) introducing reducing gas, heating to 600 ℃ at the speed of 3 ℃/min to activate the platinum alumina catalyst for 3h, and naturally cooling to room temperature; the volume ratio of the reducing gas is 1: 800 parts per million of hydrogen chloride gas and hydrogen gas mixed with pyridine vapor, wherein the hydrogen gas is mixed with 150ppm of pyridine vapor;
(3) introducing water from the bottom of the reaction tube, wetting the platinum alumina catalyst, heating by microwave under 650W, heating to 90 ℃ at the speed of 1 ℃/min, keeping the catalyst fixed, introducing hydrogen chloride gas and 20wt% sodium percarbonate solution from the bottom of the reaction tube, and reacting for 2 h; the volume ratio of the hydrogen chloride gas to the sodium percarbonate solution is 200: 1, the volume ratio of the sodium percarbonate solution to the platinum alumina catalyst is 6.5: 1;
(4) discharging the reacted gas at the top of the reaction tube, condensing and refluxing the gas into the reaction tube, and discharging the uncondensed gas after removing hydrogen chloride by alkali washing; leaching metal platinum ions in the reacted liquid, discharging the reacted liquid from the top of the reaction tube, and collecting the liquid for later use; the residual solid in the reaction tube is recycled after being washed and dried;
the content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier are detected, and the results are shown in table 3;
TABLE 3 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Example 4
The platinum alumina catalyst used was a platinum reforming catalyst with a platinum content of 0.3wt%, wherein the physical parameters of the alumina support prior to preparation of the platinum alumina catalyst were as follows: the specific surface area is 91.7m2The pore volume is 0.675mL/g, the pore diameter is 29.4nm, and the crushing strength is 37.7N; a platinum alumina catalyst having a platinum content of 0.3 wt.% and a specific surface area of 91.2m was prepared2Per g, pore volume of 0.667mL/g, pore diameter of 28.9nm, crush strength of 37.1N
The method for leaching the metal platinum in the platinum alumina catalyst by adopting a wet method is the same as the example 1;
the content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier are detected, and the results are shown in table 4;
TABLE 4 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Example 5
The platinum alumina catalyst used was a platinum reforming catalyst having a platinum content of 0.1wt%, wherein the alumina support physically participated inThe same as in example 4, a platinum alumina catalyst having a platinum content of 0.1wt% and a specific surface area of 91.5m was prepared2The pore volume is 0.676mL/g, the pore diameter is 29.3nm, and the crushing strength is 37.2N;
the method for leaching the metal platinum in the platinum alumina catalyst by adopting a wet method is the same as the example 2;
the content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier were measured, and the results are shown in table 5;
TABLE 5 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Example 6
The platinum alumina catalyst used was a platinum reforming catalyst having a platinum content of 0.5wt%, wherein the physical parameters of the alumina carrier were the same as those of example 4, and a platinum alumina catalyst having a platinum content of 0.5wt% and a specific surface area of 91.6m was prepared2The pore volume is 0.676mL/g, the pore diameter is 29.6nm, and the crushing strength is 37.4N;
the method for leaching the metal platinum in the platinum alumina catalyst by adopting a wet method is the same as the example 3;
the content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier were measured, and the results are shown in table 6;
TABLE 6 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Example 7
The adopted platinum alumina catalyst is a platinum alumina catalyst with platinum content of 5wt%, wherein the physical parameters of the alumina carrier before being prepared into the platinum alumina catalyst are as follows: the specific surface area is 314.4m2The pore volume is 0.492mL/g, the pore diameter is 6.2nm, and the crushing strength is 29.5N; preparation of a platinum alumina catalyst having a platinum content of 5wt%Agent having a specific surface area of 311.7m2The pore volume is 0.481mL/g, the pore diameter is 6.3nm, and the crushing strength is 29.4N; the method for leaching the metal platinum in the platinum alumina catalyst by adopting a wet method is the same as the example 1;
the content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier were measured, and the results are shown in table 7;
TABLE 7 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Example 8
The platinum alumina catalyst used was a platinum alumina catalyst having a platinum content of 1wt%, wherein the alumina support had the same physical parameters as in example 7, and a platinum alumina catalyst having a platinum content of 1wt% was prepared, and had a specific surface area of 313.2 m2The pore volume is 0.49mL/g, the pore diameter is 6.4 nm, and the crushing strength is 30.1N;
the method for leaching the metal platinum in the platinum alumina catalyst by adopting a wet method is the same as the example 2;
the content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier were measured, and the results are shown in table 8;
TABLE 8 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Example 9
The platinum alumina catalyst used was a platinum alumina catalyst having a platinum content of 10wt%, wherein the alumina support had the same physical parameters as in example 7, and a platinum alumina catalyst having a platinum content of 10wt% was prepared, and had a specific surface area of 308.1m2The specific surface area of the porous material is 0.459mL/g, the pore diameter is 7.1 nm, and the crushing strength is 30.2N;
the method for leaching the metal platinum in the platinum alumina catalyst by adopting a wet method is the same as the example 3;
the content, specific surface area, pore volume, pore diameter and crushing strength of platinum in the recovered alumina carrier were measured, and the results are shown in table 9;
TABLE 9 recovery of platinum metal and physical parameters of alumina carrier before and after leaching of platinum metal
Claims (10)
1. A method for leaching metal platinum in a platinum alumina catalyst by a wet method is characterized by comprising the following steps: the method comprises the following steps:
(1) filling the platinum alumina catalyst into a reaction tube of a fixed bed reactor, and then replacing air in the reaction tube with nitrogen;
(2) introducing reducing gas, heating to the temperature of 300-600 ℃, activating the platinum alumina catalyst for 3-6h, and naturally cooling to the room temperature; the reducing gas is hydrogen chloride gas and hydrogen mixed with pyridine steam;
(3) introducing water from the bottom of the reaction tube, wetting the platinum alumina catalyst, heating by microwave to 60-90 ℃, continuously maintaining the temperature, keeping the catalyst fixed, introducing hydrogen chloride gas and 10-20wt% of sodium percarbonate solution from the bottom of the reaction tube, and reacting for 2-5 h;
(4) discharging the reacted gas at the top of the reaction tube, condensing and refluxing the gas into the reaction tube, and discharging the uncondensed gas after removing hydrogen chloride by alkali washing; discharging the reacted liquid from the top of the reaction tube, and collecting for later use; and the residual solid in the reaction tube is recycled after being washed and dried.
2. The method for wet leaching platinum metal from a platinum alumina catalyst as claimed in claim 1, wherein: the platinum alumina catalyst is a platinum alumina catalyst for recovering alkane dehydrogenation with platinum content of 0.1-0.5wt%, or a platinum reforming catalyst with platinum content of 0.1-0.5wt%, or a platinum alumina catalyst with platinum content of 1-10 wt%.
3. The method for wet leaching metallic platinum from a platinum alumina catalyst as claimed in claim 1 or 2, wherein: the hydrogen gas is mixed with 50-150ppm of pyridine steam, and the volume ratio of the hydrogen chloride gas to the hydrogen gas mixed with the pyridine steam is 1: (600-800).
4. The method for wet leaching platinum metal from a platinum alumina catalyst as claimed in claim 3, wherein: the rate of temperature rise in the step (2) is 1-3 ℃/min.
5. The method for wet leaching metallic platinum from a platinum alumina catalyst as claimed in claim 1 or 2, wherein: the volume ratio of the hydrogen chloride gas to the sodium percarbonate solution in the step (3) is (100-) -200: 1, the volume ratio of the sodium percarbonate solution to the platinum alumina catalyst is (3-6.5): 1.
6. the method for wet leaching platinum metal from a platinum alumina catalyst as claimed in claim 5, wherein: the rate of microwave heating temperature rise is 0.5-1 ℃/min.
7. The method for wet leaching platinum metal from a platinum alumina catalyst as claimed in claim 5, wherein: the power of the microwave heating is 500-650W.
8. The method for wet leaching metallic platinum from a platinum alumina catalyst as claimed in claim 1 or 2, wherein: the volume ratio of the flow of the nitrogen to the platinum alumina is (0.2-0.3L/min): 1L of the compound.
9. The method for wet leaching metallic platinum from a platinum alumina catalyst as claimed in claim 1 or 2, wherein: in the step (1), the reaction tube is a quartz glass reaction tube.
10. The method for wet leaching metallic platinum from a platinum alumina catalyst as claimed in claim 1 or 2, wherein: in the step (1), the fixed bed reactor is an overflow bed reactor, and the adopted elution mode is plug flow.
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