CN101476044A - Method for recycling platinum and rhodium from binary aqua regia insoluble slag - Google Patents
Method for recycling platinum and rhodium from binary aqua regia insoluble slag Download PDFInfo
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Abstract
The invention relates to a precious-metal recovery method, specifically relates to a method of recovering platinum/rhodium from insoluble residue of dualistic royal water for solving problems of the existing platinum/rhodium recovering method that the process flow is lengthy and complicated, operational process is dangerous, the isolation effect is bad, and the like. The method comprises steps of preprocessing the insoluble residue of royal water by using barium superoxide, oxidizing the platinum and rhodium thereof, dissolving the oxidized platinum and rhodium in hydrochloric acid; using ammonium chloride to deposit platinum after being converted to a sodium type, adding hydrazine hydrate for recovering the spongy platinum, complexing by adding sodium nitrite into the filter liquor after platinum deposition, depositing rhodium by using ammonium chloride, adding hydrochloric acid for dissolving and sodium type conversion, eliminating base metal in the liquid by using ion exchange resin, finally using hydrazine hydrate and hydrogen gas flame for recovering rhodium powder. The method is a precious-metal-resource secondary recovery utilization and purification method, and has advantages of simple technique, short purification period, convenient operations, high coefficient of recovery, little discharging of waste gas and waste matter, and environment protection, and the like.
Description
Technical field
The present invention relates to a kind of precious metal recovery method, be specially a kind of method that from binary aqua regia insoluble slag, reclaims the platinum rhodium.
Background technology
In modern nitric acid industry, the method for preparing nitric acid all adopts the oxidation proceses of ammonia of your moral invention of Oswald, and promptly ammonia and Air mixing gas react under the effect of high temperature (780-950 ℃), high pressure (1-9 normal atmosphere) and catalyzer and generates NO
2, water absorbs and obtains nitric acid.Platinum and platinum rhodium catalysis net are the preferred material of nitric acid industry with catalyzer, and catalysis net used after 3-6 months, the catalysis net that loses activity and need more renew.Used do not have the main at present employing wet chemical of active platinum rhodium binary alloy catalysis net to purify, it is aqua regia dissolution that a processing step is arranged in the chemical purification process, have some black powder shape materials not dissolve in this step, we are referred to as " aqua regia insoluble slag ".Show that by analysis the composition of this aqua regia insoluble slag mainly is a Noble Metal Rhodium, also have a spot of platinum, also have some impurity elements in addition, so people are referred to as " binary aqua regia insoluble slag " usually.The annual nitric acid production in the whole nation is about 4 tons with the catalysis net loading level, if all adopt wet chemical purification platinum rhodium, estimate that the annual whole nation can produce about aqua regia insoluble slag 20-40 kilogram, according to rhodium content 80% calculating in 2000 yuan of the average prices of rhodium in 2007/gram and the insoluble slag, approximately amount to Renminbi 3200-6400 ten thousand yuan.The country that the platinum metals reserves are maximum in the world is followed successively by South Africa, Russia, Canada and the U.S. in addition, and the reserves of these four countries account for more than 95% of the whole world.China's platinum metals mineral products scarcity of resources, proven reserve only account for 3/10000ths of world saving, the Mineral resources wretched insufficiency.Along with expanding economy, supply falls short of demand in the world market platinum metals, and therefore price rises steadily in recent years.Therefore, reclaim purification rhodium and platinum and have the very important meaning that gets from the waste material of aqua regia insoluble slag or other platiniferous rhodium, it can accelerate the turnover of limited resources in industrial application, can obtain bigger economic benefit again.
The separation purification of aqua regia insoluble slag or thick rhodium powder at present is the difficult problem in the hydrometallurgy always.Traditional insoluble slag treatment process adopts zinc or aluminium to become alloy with the precious metal high-temperature fusion mostly, and hydrochloric acid is removed base metal, handles changing solution over to then with chlorination process, sal enixum or alkali fusion, and also useful pressure reduction method is handled insoluble slag.Shortcomings such as these methods not only exist technical process tediously long, numerous and diverse, and are higher to equipment requirements, and have certain risk in the operating process, and work situation is poor, separating effect is bad.
Summary of the invention
The present invention adopts traditional method in order to solve the existing platinum rhodium that reclaims from aqua regia insoluble slag, have that technical process is tediously long, numerous and diverse, equipment requirements is high, operating process is than problems such as danger and separating effect are bad, and a kind of method that reclaims the platinum rhodium from binary aqua regia insoluble slag is provided.
The present invention adopts following technical scheme to realize: a kind of method that reclaims the platinum rhodium from binary aqua regia insoluble slag may further comprise the steps:
(1) pre-treatment: binary aqua regia insoluble slag and barium peroxide is even according to the weight ratio thorough mixing of 1:4.2-6.5, then with mixture 800-950 ℃ of roasting, add dissolving with hydrochloric acid after the cooling; This step is with barium peroxide the noble metal platinum rhodium to be oxidized to available hydrochloric acid dissolved oxide compound;
(2) change the sodium type: in above-mentioned solution, add and be equivalent to precious metal weight 0.6-0.7 sodium-chlor doubly, boil the back thin up to 30-50g/L; The oxygenate conversion of above-mentioned precious metal is become the sodium type, and character is more stable;
(3) producing of spongy platinum: in above-mentioned solution, add solid ammonium chloride precipitation platinum, add-on needs 50-60 gram ammonium chloride to calculate by 100 gram platinum, fully react after-filtration, the yellow mercury oxide that produces washs with the 5-10% ammonium chloride solution, then throw out is put into pure water, 1 kilogram of throw out adds 70-90 and rises pure water, add hydrazine hydrate reduction platinum after being heated to 85-95 ℃, 1 gram platinum needs 0.65-0.8 milliliter hydrazine hydrate, the black powder that reduction reaction is generated filters, pure water is washed till neutrality, and the oven dry back got spongy platinum at 750-900 ℃ of following sintering 2-3 hour after the cooling;
(4) complexing: will add filtrate thin up that ammonium chloride reaction after-filtration obtains in the step (3), be heated to after 80-90 ℃ sodium nitrite solution complexing, complexing terminal point pH to 5-6, cooled and filtered with 450-550g/L to 30-50g/L; Obtain containing the complex compound of Noble Metal Rhodium;
(5) precipitation rhodium: the complex liquid after will filtering is put into ice bath and is cooled off, and adds the chloride precipitation rhodium, and add-on restrains rhodiums by 100 needs 140-188 gram ammonium chloride to calculate, and generates white depositions, then throw out is washed with the 5-10% ammonium chloride solution;
(6) rhodium liquid is produced: with the above-mentioned white depositions dissolving with hydrochloric acid that obtains, add in solution then and be equivalent to rhodium weight 0.6-0.7 sodium-chlor doubly;
(7) base metal in the removal solution: pH to 1-3.5 is regulated with sodium hydroxide in above-mentioned solution filtration back, and the flow velocity with the 100-150 ml/min flows through storng-acid cation exchange resin then, removes the base metal in the solution;
(8) producing of rhodium powder: directly reduce rhodium with hydrazine hydrate after the solution of above-mentioned removal base metal is heated to 85-95 ℃, 1 gram rhodium needs 1-3 milliliter hydrazine hydrate, complete reductive rhodium black is filtered, pure water is washed till neutrality, change crucible after the oven dry over to, heated 1-2 hour down, take out and grind to form powdery at 800-900 ℃, with the hydrogen flame reduction, obtain the rhodium powder then.
Compared with prior art; the present invention with binary aqua regia insoluble slag through with the barium peroxide fusion after; with noble metal platinum; rhodium is oxidized to soluble oxide compound; directly dissolve with hydrochloric acid; use chloride precipitation method separating platinum and rhodium then, get platinum, precipitate rhodium with the chloride precipitation method after the filtrate usefulness sodium nitrite solution complexing with rhodium-containing then with hydrazine hydrate reduction; change the sodium type and get rhodium liquid; spent ion exchange resin is removed base metal again, last hydrazine hydrate; hydrogen flame reduce the rhodium powder, rhodium powder purity reaches 99.95%; this is a kind of precious metal resource secondary recovery utilization and method of purification; it is simple to have technology, and the purification cycle is short, and is easy to operate; rate of recovery advantages of higher; and the waste gas and wastes discharging is few, helps protecting environment, operator's good work environment; security is good, and is simple to equipment requirements.
Embodiment
Embodiment 1:
A kind of method that from binary aqua regia insoluble slag, reclaims the platinum rhodium, may further comprise the steps: (1) pre-treatment: binary aqua regia insoluble slag and barium peroxide is even according to the weight ratio thorough mixing of 1:4.2, then with mixture 800 ℃ of roastings, add dissolving with hydrochloric acid after the cooling; (2) change the sodium type: in above-mentioned solution, add the sodium-chlor that is equivalent to 0.6 times of precious metal weight, boil the back thin up to 30g/L; (3) producing of spongy platinum: in above-mentioned solution, add solid ammonium chloride precipitation platinum, add-on needs 50 gram ammonium chlorides to calculate by 100 gram platinum, heating is also fully reacted after-filtration, the yellow mercury oxide that produces washs with 5% ammonium chloride solution, then throw out is put into pure water, 1 kilogram of throw out adds 70 liters of pure water, add hydrazine hydrate reduction platinum after being heated to 85 ℃, 1 gram platinum needs 0.65 milliliter of hydrazine hydrate, the black powder that reduction reaction is generated filters, pure water is washed till neutrality, and oven dry back is 750 ℃ of following sintering 2 hours, after the cooling spongy platinum; (4) complexing: will add filtrate thin up that ammonium chloride reaction after-filtration obtains in the step (3), be heated to after 80 ℃ sodium nitrite solution complexing, complexing terminal point pH to 5, cooled and filtered with 450g/L to 30g/L; (5) precipitation rhodium: the complex liquid after will filtering is put into ice bath and is cooled off, and adds the chloride precipitation rhodium, and add-on needs 140 gram ammonium chlorides to calculate by 100 gram rhodiums, generates white depositions, then throw out is washed with 5% ammonium chloride solution; (6) rhodium liquid is produced: with the above-mentioned white depositions dissolving with hydrochloric acid that obtains, add the sodium-chlor that is equivalent to 0.6 times of rhodium weight then in solution; (7) base metal in the removal solution: pH to 1 is regulated with sodium hydroxide in above-mentioned solution filtration back, and the flow velocity with 100 ml/min flows through storng-acid cation exchange resin then, removes the base metal in the solution; (8) producing of rhodium powder: directly reduce rhodium with hydrazine hydrate after the solution of above-mentioned removal base metal is heated to 85 ℃, 1 gram rhodium needs 1 milliliter of hydrazine hydrate, complete reductive rhodium black is filtered, pure water is washed till neutrality, change crucible after the oven dry over to, heated 1 hour down, take out and grind to form powdery at 800 ℃, with the hydrogen flame reduction, obtain the rhodium powder then.
Handle the binary aqua regia insoluble slag contain platinum 4.37% and rhodium 80.58% with this method, how many rate of recovery of platinum is 97.3%, and the rate of recovery of rhodium is 97.5%, makes purity and be 99.95% platinum powder and purity and be 99.98% rhodium powder.
Embodiment 2:
A kind of method that from binary aqua regia insoluble slag, reclaims the platinum rhodium, may further comprise the steps: (1) pre-treatment: binary aqua regia insoluble slag and barium peroxide is even according to the weight ratio thorough mixing of 1:6.5, then with mixture 950 ℃ of roastings, add dissolving with hydrochloric acid after the cooling; (2) change the sodium type: in above-mentioned solution, add the sodium-chlor that is equivalent to 0.7 times of precious metal weight, boil the back thin up to 50g/L; (3) producing of spongy platinum: in above-mentioned solution, add solid ammonium chloride precipitation platinum, add-on needs 60 gram ammonium chlorides to calculate by 100 gram platinum, heating is also fully reacted after-filtration, the yellow mercury oxide that produces washs with 10% ammonium chloride solution, then throw out is put into pure water, 1 kilogram of throw out adds 90 liters of pure water, add hydrazine hydrate reduction platinum after being heated to 95 ℃, 1 gram platinum needs 0.8 milliliter of hydrazine hydrate, the black powder that reduction reaction is generated filters, pure water is washed till neutrality, and oven dry back is 900 ℃ of following sintering 3 hours, after the cooling spongy platinum; (4) complexing: will add filtrate thin up that ammonium chloride reaction after-filtration obtains in the step (3), be heated to after 90 ℃ sodium nitrite solution complexing, complexing terminal point pH to 6, cooled and filtered with 550g/L to 50g/L; (5) precipitation rhodium: the complex liquid after will filtering is put into ice bath and is cooled off, and adds the chloride precipitation rhodium, and add-on needs 188 gram ammonium chlorides to calculate by 100 gram rhodiums, generates white depositions, then throw out is washed with 10% ammonium chloride solution; (6) rhodium liquid is produced: with the above-mentioned white depositions dissolving with hydrochloric acid that obtains, add the sodium-chlor that is equivalent to 0.7 times of rhodium weight then in solution; (7) base metal in the removal solution: pH to 3.5 is regulated with sodium hydroxide in above-mentioned solution filtration back, and the flow velocity with 150 ml/min flows through storng-acid cation exchange resin then, removes the base metal in the solution; (8) producing of rhodium powder: directly reduce rhodium with hydrazine hydrate after the solution of above-mentioned removal base metal is heated to 95 ℃, 1 gram rhodium needs 3 milliliters of hydrazine hydrates, complete reductive rhodium black is filtered, pure water is washed till neutrality, change crucible after the oven dry over to, heated 2 hours down, take out and grind to form powdery at 900 ℃, with the hydrogen flame reduction, obtain the rhodium powder then.
Handle the binary aqua regia insoluble slag contain platinum 2.45% and rhodium 76.6% with this method, how many rate of recovery of platinum is 96.45%, and the rate of recovery of rhodium is 96.28%, makes purity and be 99.96% platinum powder and purity and be 99.95% rhodium powder.
Embodiment 3:
A kind of method that from binary aqua regia insoluble slag, reclaims the platinum rhodium, may further comprise the steps: (1) pre-treatment: binary aqua regia insoluble slag and barium peroxide is even according to the weight ratio thorough mixing of 1:4.2, then with mixture 950 ℃ of roastings, add dissolving with hydrochloric acid after the cooling; (2) change the sodium type: in above-mentioned solution, add the sodium-chlor that is equivalent to 0.6 times of precious metal weight, boil the back thin up to 40g/L; (3) producing of spongy platinum: in above-mentioned solution, add solid ammonium chloride precipitation platinum, add-on needs 50 gram ammonium chlorides to calculate by 100 gram platinum, heating is also fully reacted after-filtration, the yellow mercury oxide that produces washs with 7% ammonium chloride solution, then throw out is put into pure water, 1 kilogram of throw out adds 70 liters of pure water, add hydrazine hydrate reduction platinum after being heated to 90 ℃, 1 gram platinum needs 0.65 milliliter of hydrazine hydrate, the black powder that reduction reaction is generated filters, pure water is washed till neutrality, and oven dry back is 900 ℃ of following sintering 2 hours, after the cooling spongy platinum; (4) complexing: will add filtrate thin up that ammonium chloride reaction after-filtration obtains in the step (3), be heated to after 85 ℃ sodium nitrite solution complexing, complexing terminal point pH to 6, cooled and filtered with 450g/L to 45g/L; (5) precipitation rhodium: the complex liquid after will filtering is put into ice bath and is cooled off, and adds the chloride precipitation rhodium, and add-on needs 155 gram ammonium chlorides to calculate by 100 gram rhodiums, generates white depositions, then throw out is washed with 8% ammonium chloride solution; (6) rhodium liquid is produced: with the above-mentioned white depositions dissolving with hydrochloric acid that obtains, add the sodium-chlor that is equivalent to 0.7 times of rhodium weight then in solution; (7) base metal in the removal solution: pH to 2 is regulated with sodium hydroxide in above-mentioned solution filtration back, and the flow velocity with 120 ml/min flows through storng-acid cation exchange resin then, removes the base metal in the solution; (8) producing of rhodium powder: directly reduce rhodium with hydrazine hydrate after the solution of above-mentioned removal base metal is heated to 95 ℃, 1 gram rhodium needs 2 milliliters of hydrazine hydrates, complete reductive rhodium black is filtered, pure water is washed till neutrality, change crucible after the oven dry over to, heated 2 hours down, take out and grind to form powdery at 800 ℃, with the hydrogen flame reduction, obtain the rhodium powder then.
Handle the binary aqua regia insoluble slag contain platinum 5.73% and rhodium 78.34% with this method, how many rate of recovery of platinum is 95.63%, and the rate of recovery of rhodium is 96.13%, makes purity and be 99.95% platinum powder and purity and be 99.97% rhodium powder.
Embodiment 4:
A kind of method that from binary aqua regia insoluble slag, reclaims the platinum rhodium, may further comprise the steps: (1) pre-treatment: binary aqua regia insoluble slag and barium peroxide is even according to the weight ratio thorough mixing of 1:5.0, then with mixture 850 ℃ of roastings, add dissolving with hydrochloric acid after the cooling; (2) change the sodium type: in above-mentioned solution, add the sodium-chlor that is equivalent to 0.6 times of precious metal weight, boil the back thin up to 35g/L; (3) producing of spongy platinum: in above-mentioned solution, add solid ammonium chloride precipitation platinum, add-on needs 55 gram ammonium chlorides to calculate by 100 gram platinum, heating is also fully reacted after-filtration, the yellow mercury oxide 7% ammonium chloride solution washing that produces, then throw out is put into pure water, 1 kilogram of throw out adds 85 liters of pure water, add hydrazine hydrate reduction platinum after being heated to 88 ℃, 1 gram platinum needs 0.75 milliliter of hydrazine hydrate, the black powder that reduction reaction is generated filters, pure water is washed till neutrality, and oven dry back is 850 ℃ of following sintering 2.5 hours, after the cooling spongy platinum; (4) complexing: will add filtrate thin up that ammonium chloride reaction after-filtration obtains in the step (3), be heated to after 90 ℃ sodium nitrite solution complexing, complexing terminal point pH to 5, cooled and filtered with 525g/L to 35g/L; (5) precipitation rhodium: the complex liquid after will filtering is put into ice bath and is cooled off, and adds the chloride precipitation rhodium, and add-on needs 165 gram ammonium chlorides to calculate by 100 gram rhodiums, generates white depositions, then throw out is washed with 6% ammonium chloride solution; (6) rhodium liquid is produced: with the above-mentioned white depositions dissolving with hydrochloric acid that obtains, add the sodium-chlor that is equivalent to 0.6 times of rhodium weight then in solution; (7) base metal in the removal solution: pH to 3.0 is regulated with sodium hydroxide in above-mentioned solution filtration back, and the flow velocity with 140 ml/min flows through storng-acid cation exchange resin then, removes the base metal in the solution; (8) producing of rhodium powder: directly reduce rhodium with hydrazine hydrate after the solution of above-mentioned removal base metal is heated to 90 ℃, 1 gram rhodium needs 2 milliliters of hydrazine hydrates, complete reductive rhodium black is filtered, pure water is washed till neutrality, change crucible after the oven dry over to, heated 1.5 hours down, take out and grind to form powdery at 870 ℃, with the hydrogen flame reduction, obtain the rhodium powder then.
Handle the binary aqua regia insoluble slag contain platinum 6.83% and rhodium 76.52% with this method, how many rate of recovery of platinum is 95.78%, and the rate of recovery of rhodium is 95.93%, makes purity and be 99.97% platinum powder and purity and be 99.95% rhodium powder.
Claims (1)
1, a kind of method that reclaims the platinum rhodium from binary aqua regia insoluble slag is characterized in that may further comprise the steps:
(1) pre-treatment: binary aqua regia insoluble slag and barium peroxide is even according to the weight ratio thorough mixing of 1:4.2-6.5, then with mixture 800-950 ℃ of roasting, add dissolving with hydrochloric acid after the cooling;
(2) change the sodium type: in above-mentioned solution, add and be equivalent to precious metal weight 0.6-0.7 sodium-chlor doubly, boil the back thin up to 30-50g/L;
(3) producing of spongy platinum: in above-mentioned solution, add solid ammonium chloride precipitation platinum, add-on needs 50-60 gram ammonium chloride to calculate by 100 gram platinum, heating is also fully reacted after-filtration, the yellow mercury oxide that produces washs with the 5-10% ammonium chloride solution, then throw out is put into pure water, 1 kilogram of throw out adds 70-90 and rises pure water, add hydrazine hydrate reduction platinum after being heated to 85-95 ℃, 1 gram platinum needs 0.65-0.8 milliliter hydrazine hydrate, the black powder that reduction reaction is generated filters, pure water is washed till neutrality, and the oven dry back got spongy platinum at 750-900 ℃ of following sintering 2-3 hour after the cooling;
(4) complexing: will add filtrate thin up that ammonium chloride reaction after-filtration obtains in the step (3), be heated to after 80-90 ℃ sodium nitrite solution complexing, complexing terminal point pH to 5-6, cooled and filtered with 450-550g/L to 30-50g/L;
(5) precipitation rhodium: the complex liquid after will filtering is put into ice bath and is cooled off, and adds the chloride precipitation rhodium, and add-on restrains rhodiums by 100 needs 140-188 gram ammonium chloride to calculate, and generates white depositions, then throw out is washed with the 5-10% ammonium chloride solution;
(6) rhodium liquid is produced: with the above-mentioned white depositions dissolving with hydrochloric acid that obtains, add in solution then and be equivalent to rhodium weight 0.6-0.7 sodium-chlor doubly;
(7) base metal in the removal solution: pH to 1-3.5 is regulated with sodium hydroxide in above-mentioned solution filtration back, and the flow velocity with the 100-150 ml/min flows through storng-acid cation exchange resin then, removes the base metal in the solution;
(8) producing of rhodium powder: directly reduce rhodium with hydrazine hydrate after the solution of above-mentioned removal base metal is heated to 85-95 ℃, 1 gram rhodium needs 1-3 milliliter hydrazine hydrate, complete reductive rhodium black is filtered, pure water is washed till neutrality, change crucible after the oven dry over to, heated 1-2 hour down, take out and grind to form powdery at 800-900 ℃, with the hydrogen flame reduction, obtain the rhodium powder then.
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| CN114657381B (en) * | 2022-03-17 | 2023-10-31 | 金川集团股份有限公司 | Method for recovering rhodium from waste liquid of production of rhodium acetylacetonate triphenylphosphine carbonyl |
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