A kind of method reclaiming platinum from spent catalyst
Technical field
The present invention relates to noble metal catalyst and reclaim field, especially a kind of method reclaiming platinum from spent catalyst.
Background technology
The range of application of platinum metals is extremely wide, is called as " modern industry vitamin b6 usp " and " the first high-technology metal ".Wherein platinum is most widely used, consumption is maximum.Be mainly used in chemistry, petrochemical complex catalyzer; Motor car exhaust gas catalysis purifies; Platinum ornaments; Temperature element; Glass, fiber glass industry crucible, bushing etc.
1875, since taking platinum as the process industry of contact process manufacture sulfuric acid of catalyzer, the industrial application of noble metal catalyst emerged in an endless stream.1913, platinum catalysis net was used for preparing nitric acid by ammonia oxidation; Nineteen thirty-seven, Ag/Al
2o
3catalyzer is used for oxidation of ethylene epoxy ethane; 1949, Pt/Al
2o
3catalyzer is used for petroleum reforming and produces high-quality gasoline; Nineteen fifty-nine, PdCl
2-CuCl
2catalyzer is used for oxidation of ethylene acetaldehyde; To late 1960s, there is again synthesizing acetic acid by methanol low-pressure carbonylation rhodium complex catalyst.Most catalyzer is the catalyzer of load highly disperse active metal on porous inorganic carrier.Shape has particulate state, spherical, column, sheet or cellular etc.
Since two thousand three, the application of platinum presents the situation that supply falls short of demand, and the platinum content in catalyzer is far away higher than the content of platinum in mineral reserve, and therefore spent catalyst becomes very important platinum secondary resource, has high recovery value.Existing recovery method mainly contains: mechanically peel method, and the consumption of this method reagent is few, becomes local, but metal dispersion, and technology difficulty is large; Smelting process, this kind of simple cost of method is low, but the rate of recovery is not high, and energy consumption is large; Carrier solubilizes method, this kind of method is simple, but reagent consumption is large, and higher to equipment requirements.
Summary of the invention
For solving the deficiencies in the prior art, the object of this invention is to provide a kind of method reclaiming platinum from inactive noble metal catalyst, possessing skills simple, the advantages such as easy to operate, the rate of recovery is high, agents useful for same reusable edible.
The present invention is achieved through the following technical solutions:
From spent catalyst, reclaim a method for platinum, it is characterized in that, comprise the following steps:
1) grind, spent catalyst is ground to form fine particle;
2) make charcoal, by the spent catalyst roasting 1h after grinding, maturing temperature is 400 ~ 600 DEG C;
3) wet-milling, seal wet-milling by putting into autoclave through the spent catalyst of above-mentioned process and abrasive mixing, the ratio of described catalyzer and abrasive is 8 ~ 10:1;
4) leach, wet ground final vacuum suction filtration, by solid-liquid separation, leached mud and leach liquor put into autoclave jointly, pressurized, heated;
5) essence is purified.
Further, described step 3) wet-milling temperature is 150 ~ 200 degrees Celsius, and reaches a timing in temperature, in still, blast oxygen.
Further, described step 3) abrasive is sodium hydroxide in wet-milling.
Further, described step 4) leach described in leach liquor be 5% ~ 10% NaCN solution.
Further, described step 4) leach described in leach liquor be 7% NaCN solution.
Further, described step 4) leach described in Heating temperature be 140 ~ 160 DEG C, pressure is 1.6 ~ 2MPa.
Further, what blast in still is pure oxygen.
Beneficial effect: compared with existing recovery method, the present invention eliminates this step acid-soluble in removal process, has saved cost, reduces equipment loss, reduces disposal of three wastes expense, finally reaches reduction production cost, reduces the object of production cycle.
Embodiment
In order to make technique means of the present invention, creation characteristic, reach object and effect is easy to understand, below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment 1
Spent catalyst grinds to form fine particle, spent catalyst after grinding is put into retort furnace roasting 1h, maturing temperature is 400 DEG C, after cooling, seal wet-milling by putting into autoclave through the spent catalyst of above-mentioned process and the mixing of abrasive sodium hydroxide, the ratio of catalyzer and abrasive is 8:1, and wet-milling temperature is 150 DEG C, and when temperature reaches 140 DEG C, in still, blast oxygen.Raw material after wet ground is through vacuum filtration, and by solid-liquid separation, leached mud and leach liquor put into autoclave jointly, and leach liquor is the NaCN solution of 5%, and leaching Heating temperature is 140 DEG C, and pressure is 1.6MPa, and recording platinum leaching yield after cooling is 90%.
Embodiment 2
Spent catalyst grinds to form fine particle, spent catalyst after grinding is put into retort furnace roasting 1h, maturing temperature is 400 DEG C, after cooling, seal wet-milling by putting into autoclave through the spent catalyst of above-mentioned process and the mixing of abrasive sodium hydroxide, the ratio of catalyzer and abrasive is 8:1, and wet-milling temperature is 170 DEG C, and when temperature reaches 160 DEG C, in still, blast oxygen.Raw material after wet ground is through vacuum filtration, and by solid-liquid separation, leached mud and leach liquor put into autoclave jointly, and leach liquor is the NaCN solution of 5%, and leaching Heating temperature is 160 DEG C, and pressure is 2MPa, and recording platinum leaching yield after cooling is 94%.
Embodiment 3
Spent catalyst grinds to form fine particle, spent catalyst after grinding is put into retort furnace roasting 1h, maturing temperature is 500 DEG C, after cooling, seal wet-milling by putting into autoclave through the spent catalyst of above-mentioned process and the mixing of abrasive sodium hydroxide, the ratio of catalyzer and abrasive is 10:1, and wet-milling temperature is 200 DEG C, and when temperature reaches 170 DEG C, in still, blast oxygen.Raw material after wet ground is through vacuum filtration, and by solid-liquid separation, leached mud and leach liquor put into autoclave jointly, and leach liquor is the NaCN solution of 7%, and leaching Heating temperature is 140 DEG C, and pressure is 1.6 ~ 2MPa, and recording platinum leaching yield after cooling is 93%.
Embodiment 4
Spent catalyst grinds to form fine particle, spent catalyst after grinding is put into retort furnace roasting 1h, maturing temperature is 600 DEG C, after cooling, seal wet-milling by putting into autoclave through the spent catalyst of above-mentioned process and the mixing of abrasive sodium hydroxide, the ratio of catalyzer and abrasive is 10:1, and wet-milling temperature is 200 DEG C, and when temperature reaches 175 DEG C, in still, blast oxygen.Raw material after wet ground is through vacuum filtration, and by solid-liquid separation, leached mud and leach liquor put into autoclave jointly, and leach liquor is the NaCN solution of 10%, and leaching Heating temperature is 160 DEG C, and pressure is 2MPa, and recording platinum leaching yield after cooling is 95%.