Method of separation of metallic palladium from waste mangani-palladium catalyst

FIELD: separation of palladium from waste mangani-palladium catalyst and cleaning of palladium.

SUBSTANCE: palladium-containing concentrate is treated with aqua regia solution and palladium is deposited in form of chloropalladate by means of treatment with aqua regia solution with solid ammonium chloride, pulp thus obtained is settled, cooled and filtered; sediment is treated with saturated hydrochloric acid solution of ammonium chloride. Then sediment thus treated is dissolved in water and solution is filtered and neutralized; pallarium is restored to metal by means of hydrochloric acid hydrazine at pH≥2 or formic acid solution at pH≥6; solution is filtered and metallic palladium is washed and dried at 90-100°C. Prior to treatment, mangani-palladium catalyst with aqua regia, it is dissolved in concentrated hydrochloric acid; solution is neutralized by asmmonia to pH=6-7 and treated with formic acid at flow rate no less than 1 l of HCOOH per kg of mangani-palladium catalyst; then mangani-palladium concentrate is filtered, washed and dried at 90-100ºC.

EFFECT: enhanced purity of metallic palladium at minimum losses of catalyst at all stages of chemical treatment.

4 ex

 

The invention relates to the field of isolation and purification of palladium, in particular, from spent margantsevokislogo catalyst.

A method of obtaining dichlorodiammineplatinum from spent aluminum-palladium catalyst (patent RF №2100277 IPC6C 01 11/00, 55/00), including the firing of a catalyst at 500-700°, raspulpovka in water, processing water slurry with sulfuric acid, followed by heating and diluting the resulting mixture with water, separating palladium residue, dissolving it in hydrochloric acid, the processing of hydrochloric acid solution with ammonia, and the Department of ammonia solution of palladium, the processing of hydrochloric acid and separating the resulting precipitate dichlorodiammineplatinum. The disadvantage of this method when it is used for selection of palladium in the form of a metal from spent margantsevokislogo catalyst is too long and multistage processing of the source material, which is associated with the loss of palladium. Moreover, the firing of the catalyst in a stream of air at 500-700°With palladium partially oxidized, which will require additional surgeries to repair it.

Also known hydrometallurgical method of selection of palladium containing material (RF patent No. 2096505 IPC622 In 11/00), including melting and g is the cancellation of the original material, dissolve pellet in nitric, acid, separation of impurities in the form of hydroxide, dissolving the calcined palladium residue in a solution of Aqua Regia and the deposition of palladium from a filtered solution of sodium thiosulfate. The disadvantage of this method is the duration of the processing of the source material. In addition, when using palladium isolated in the form of a practically insoluble palladium sulfide, which complicates further processing to obtain the palladium in the form of metal.

Closest to the claimed technical solution is the method of obtaining metallic palladium (RF patent No. 2210609 IPC722 In 11/01, 3/05, 3/44), including the processing of palladium material with a solution of Aqua Regia, the deposition of palladium in the form of a salt of globaldata processing tsarskovodochnom solution of ammonium chloride, defending the obtained slurry, cooling, filtering and processing the precipitate on the filter with a solution of ammonium chloride. Salt globaldata precipitated solid ammonium chloride, the precipitate on the filter is treated with saturated hydrochloric acid solution of ammonium chloride, treated residue is dissolved in water, the resulting solution is filtered, neutralized and carry out the restoration of palladium to the metal, and the metal palladium is filtered off, washed and su is at 90-100° C. the recovery of palladium metal to conduct hydrochloric acid with hydrazine at pH≥2 or formic acid at pH≥6.

The disadvantage of this method when used for production of the metallic palladium from spent margantsevokislogo catalyst is that, as determined experimentally, during the precipitation of salts of chloropalladite of tsarskovodochnom solution containing large amounts of impurities, the precipitate formed is very small, which greatly complicates its filtering off and washing and significantly reduces the efficiency of the process for producing metallic palladium.

An object of the invention is to obtain pure metallic palladium with minimum losses at all stages of chemical processing margantsevokislogo catalyst.

This object is achieved in that the palladium concentrate is treated with a solution of Aqua Regia, precipitated palladium in the form of a salt of globaldata processing tsarskovodochnom solution of solid ammonium chloride, defend and cool the resulting slurry is filtered and treated sludge on the filter nasadenim hydrochloric acid solution of ammonium chloride, dissolved processed sediment in water, filtered off and neutralize the resulting solution, restore palladium to meta the La hydrochloric acid with hydrazine at pH≥ 2 or formic acid at pH≥6, is filtered off, washed and dried metallic palladium in the 90-100°C. When the metallic palladium is obtained from spent margantsevokislogo catalyst. Before treatment with a solution of Aqua Regia exhaust margantsevorudny the catalyst is dissolved in concentrated hydrochloric acid, the solution is neutralized with ammonia to a pH of 6-7, treated with formic acid at a flow rate not less than 1 l HCOOH 1 kg margantsevokislogo catalyst, followed by filtering, washing and drying to obtain palladium concentrate at 90-100°C, which is treated with a solution of Aqua Regia.

In the claimed technical solution is proposed a method of obtaining a palladium concentrate allows you to separate the main impurities and to allocate palladium in the form of pure metal with minimal losses at all stages of chemical processing of spent margantsevokislogo catalyst.

The analysis of publicly available sources about the level of technology did not allow to identify a technical solution, identical claimed, on the basis of which a conclusion is made about the uncertainty of the latter, i.e. under provided in this application of the invention, the criterion of "novelty".

Comparative analysis of the claimed solution is Zvezdnyi technical solutions revealed that presents a set of distinctive features is not known to the person skilled in the art and not obvious from the prior art, on the basis of which a conclusion of compliance presented in this application of the invention, the criterion of "inventive step".

The proposed method of producing metallic palladium from spent margantsevokislogo catalyst implemented as follows.

Example 1.

500 g of spent margantsevokislogo catalyst containing 13 g of palladium, a large amount of manganese, as well as impurities of copper, lead, Nickel, zinc and aluminum dissolved in concentrated hydrochloric acid, the resulting solution was neutralized with ammonia to a pH of 6-7 and added 0.5 l of formic acid. Adjusted the pH of the solution by adding ammonia. The solution with the precipitate is boiled until complete discoloration of the solution. The precipitate was washed by decantation with hot water and filtered.

The palladium content in the filtrate was <0.8 mg/L. the resulting concentrate was dried at 90-100°With and dissolved in Aqua Regia. The cooled solution was added ammonium chloride ammonium in the form of a solid salt at the rate of 1 g NH4Cl 1 g of palladium and an excess of NH4CL - 10 g/L. the resulting slurry was stood for 5 hours and filtered through a filter of chlorin cloth is. The palladium content in the filtrate was 1.1 mg/l Residue on the filter was treated with hydrochloric acid (2:1) saturated ammonium chloride. The palladium content in the wash water was <0.4 mg/l Residue was dissolved in water when heated, filtered, the resulting solution was neutralized to pH 6 and added formic acid at the rate of 1.5 ml of HCOOH on 1 g of palladium. Adjusted the pH of the solution by adding ammonia. The solution is then treated with palladium was boiled before complete clarification of the solution. The precipitate was filtered, washed with hot water and dried at 90-100°C. the palladium Content in the filtrate and the wash water was 0.1 mg/L. palladium Metal was analyzed for impurities by the method of mass-spectral analysis. It was 0,0719%.

Example 2.

Metal palladium was obtained as in example 1, but in hydrochloric acid solution was added 0.6 l of formic acid. The obtained concentrate was washed, filtered, dried, dissolved in Aqua Regia, besieged salt chloropalladite, washed and dissolved it as in example 1, but the filtered solution globaldata was neutralized with ammonia to pH 2 and spent recovering palladium hydrazine hydrochloric acid, added at the rate of 1 g of N2H4·2hcl 1 g of palladium and an excess of N2H4·2hcl - 2 g/l Separation, washing and drying the obtained metallicheskogo palladium conducted as in example 1. The palladium content in arabinoxylan the filtrate was <0.8 mg/l, the content of palladium in the filtrate and the wash water after deposition and processing of salt localedata - 1.4 and 0.5 mg/l, respectively, the palladium content in the filtrate after restoring it to metal - <0.2 mg/l Total content of impurities in the resulting metal was 0,0809%.

Example 3.

Metal palladium was obtained as in example 1, but in hydrochloric acid solution was added 0.4 l of formic acid. The palladium content in the filtrate after filtration of the obtained concentrate was 103 mg/l, Filtration, washing, drying, dissolving the concentrate in Aqua Regia, the precipitation of the salt of chloropalladite, washing, dissolution, filtration, recovery of metallic palladium, washing and drying were carried out as in example 1. The palladium content in the filtrate and the wash water after deposition and processing of salt globaldata was 1.8 and 0.3 mg/l, respectively, the palladium content in the filtrate after restoring it to metal - <0.1 mg/l, the total content of impurities in the obtained metal - 0,0756%.

Example 4.

Obtaining metallic palladium held by the RF patent №2210609 IPC722 In 11/00, 3/06, 3/44 selected as the closest technical solution.

500 g of spent melaniemelanie catalyst R who has storyli in Aqua Regia when heated. In the resulting solution was added ammonium chloride in the form of a solid salt at the rate of 1 g NH4CL 1 g of palladium and an excess of NH4Cl - 10 g/L. When this NH4CL formed a tight wad and dissolve very slowly, so the resulting slurry to stand for 20 hours. Sludge globaldata formed very small and did not hoteltravel through the filter of chlorin tissue, so the precipitate was filtered by gravity through a porous glass filter (pore 41). The duration of filtration increased ˜ 100 times. The palladium content in the filtrate was < 1 mg/l Residue on the filter was treated with hydrochloric acid (2:1), saturated ammonium chloride. Leaching duration also increased ˜ 100 times. The palladium content in the wash water was <0.8 mg/l Residue was dissolved in water when heated, filtered, the resulting solution was neutralized it with ammonia to a pH of 6 and spent recovering palladium formic acid, added at the rate of 1.5 ml of HCOOH on 1 g of palladium. The solution is then treated with palladium was boiled before complete clarification of the solution. The precipitate was filtered, washed with hot water and dried at 90-100°C. the palladium Content in the filtrate and the wash water was <0.2 mg/l, the total Content of impurities in the metallic palladium was 0,0913%.

The results obtained indicated at log on is shown using the known technical solutions are compared with the proposed significantly increased the duration of the process of obtaining metallic palladium and significantly decreased its performance. In addition, for filtering off the precipitate of globaldata had to use glass, porous filters, that is to complicate the hardware design process, the proposed method of producing metallic palladium allows you to select from spent margantsevokislogo catalyst more than 99% of palladium with purification 0.07197%.

The developed method allows the use of standard equipment, cheap and available reagents, does not require large power consumption. The method is suitable from an environmental point of view, as the resulting acidic filtrates are neutralized with caustic soda solution.

Method for producing metallic palladium palladium from spent catalyst includes treatment with a solution of Aqua Regia, the deposition of palladium in the form of a salt of globaldata processing tsarskovodochnom solution of solid ammonium chloride, defending the obtained slurry, cooling, filtering and processing the precipitate on the filter is saturated hydrochloric acid solution of ammonium chloride, dissolving the treated sludge in water, filtering the resulting solution, neutralization, recovery of palladium to the metal hydrazine hydrochloric acid at pH≥2 or formic acid at pH≥6, the filter palladium metal, washing and drying at 90-100 , Characterized in that palladium metal produced from waste margantsevokislogo catalyst before the treatment with a solution of Aqua Regia exhaust margantsevorudny the catalyst is dissolved in concentrated hydrochloric acid, the solution is neutralized with ammonia to a pH of 6-7, treated with formic acid at a flow rate not less than 1 l HCOOH 1 kg margantsevokislogo catalyst, followed by filtering, washing and drying to obtain palladium concentrate at 90-100°S, which is treated with a solution of Aqua Regia.



 

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