Method for extraction of palladium (ii) from wasted catalysts

FIELD: hydrometallurgy.

SUBSTANCE: the invention relates to hydrometallurgy of precious metals and can be used to extract palladium from wasted catalysts, including catalysts of low-temperature oxidation of carbon oxide (II) based on γ-Al2O3, containing palladium chloride (II) and cupric bromide (II). The method includes acid leaching of palladium from wasted catalysts from the chloride solution. Furthermore, the acid leaching is carried out by 1 M solution of hydrochloric acid. The resulting solution is diluted with water to pH 1. The sorption of palladium is carried out from the diluted solution using chemically modified silica containing grafted groups of γ-aminopropyltriethoxysilane.

EFFECT: increased amount of extracted palladiumusing a cheap nitrogen-containing sorbent, the high speed of the process and the possibility to regenerate the sorbent.

4 tbl

 

The invention relates to the field of hydrometallurgy of precious metals and can be used for the recovery of palladium from spent catalysts, including catalysts for low temperature oxidation of carbon monoxide(II) based on γ-Al2About3containing palladium(II) chloride and copper bromide(II).

A method of refining containing metals of platinum group spent catalysts based on oxides of aluminum, silicon and magnesium, which includes processing of the crushed catalyst with a solution of sulfuric acid, sintering the insoluble residue with alkali metal hydroxide at a temperature of 400-700°C, followed by alkaline leaching of cake. Disadvantages of the method are the use of energy-intensive pyrometallurgical operations sintering, the duration of individual operations [RF patent for the invention №2138568. Gadjiev S.E., Kovtun, VA, Parecki VM and other publ. 27.09.1999].

The closest technical solution is the method of extraction of palladium from spent catalysts, the essence of which lies in the acid leaching of spent catalysts "Tsar's vodka", the process of evaporation of a solution to the dry residue and dissolving the dry residue in hydrochloric acid with subsequent sorption of palladium chloride solution on carbon sorbents [RF patent for the invention №2339712. Th is AEWA N.G., Kononova O., Dostovalov NB and other Publ. 27.11.2008]. Obtained as a result of sorption of solutes containing precious metal, it is proposed to burn.

The disadvantage of this method are the use of leaching of spent catalysts solutions "Aqua Regia", in the process of evaporation which form volatile oxides of nitrogen, the duration of the process of sorption - 24 h, the inability to regenerate the sorbent.

The technical result of the invention is to reduce the amount of harmful gas emissions, improving the performance of the process by reducing the time of sorption of palladium chloride solutions from reprocessing of spent catalysts, the possibility of sorption in the dynamic mode, as well as reusable sorbent due to desorption of palladium.

This technical result is achieved in that in the method of extraction of palladium(II) from spent catalysts, including preliminary acid leaching of palladium from spent catalysts and sorption of palladium chloride solution, followed by desorption of palladium with a solution of thiourea, acid leaching lead 1 m solution of Hcl, the solution was diluted with water to a pH of 1, and the obtained solution is performed in the sorption of palladium on chemically modified silica containing at which itie group γ aminopropyltriethoxysilane. Desorption of palladium(II) is conducted with a solution of thiourea in hydrochloric acid.

The inventive method is carried out as follows.

Exhaust catalysts for low temperature oxidation of carbon monoxide(II) based on γ-Al2About3containing palladium(II) chloride and copper bromide(II), were subjected to acid leaching of 1 M Hcl. The obtained chloride-bromide solutions containing ions of palladium(II), was diluted with water to a pH of 1 and contacted with the sorbent in static or dynamic conditions. The sorbent is a chemically modified silica-based Silochrome C-120 series VG - 102/A (specific surface area of 120 m2/g, the fraction 0.1-0.2 mm, the average diameter of pores is 45 nm)containing grafted group γ aminopropyltriethoxysilane. The preferred amount of the grafted functional groups of the sorbent is 0.5-1,63 mmol/g Initial concentration of metals in the solutions varied in the range CPd=0,43-1,60 g/l, CCu=0,89-3.11 g/l;Al=0,40-1,62 g/L. Experiments in static conditions was obtained from individual (containing ions of only one metal) hydrochloric acid solutions (0.1 M to 4 M Hcl) at room temperature, the volume of the solution was 15 ml, the mass of the sample sorbent 0,03±0,001, Experiments on sorption in the dynamic mode of the individual solutions and real, obtained by leaching the OTP is developed catalysts in 1 M Hcl, were carried out in glass columns, inner diameter of which was 0.4 cm Sample sorbents from 0.1 g to 0.2, the Passage of the solution through the column was by gravity. After adsorption sorbents were washed in 0.1 M Hcl or water, and then missed the eluent solution. Metal concentrations in the initial and final solutions were determined by the following methods: the concentration of palladium(II) - by the method with tin chloride(II) [Ginzburg, S., Ezersky N.A., Prokofiev IV and other Analytical chemistry of the elements. Platinum metals. M.: "Nauka". 1972. S], copper(II) with potassium thiocyanate [Podchaynov V.N., Anosova S. p. Journal of analytical chemistry. 1958. Volume XIII, issue 5. P.533-537], the content of palladium(II) in solutions containing copper(II)was determined by reaction with dimethylglyoxime by the method of [Michelson PB, Kalabina L.V. Extraction-spectrophotometric determination of palladium(II) dimethylglyoxime. The journal analytical chemistry. 1969. 24, issue 2. Pp.261-263.], the amount of copper in model solutions containing palladium(II), found using sodium diethyldithiocarbamate [Babaeva ST, Marking L.A., Krylov, L.P., Navassa E.A., Salova A.S. Methods for the determination of paints and varnishes. M: "Chemistry". 1974. P.472]. Aluminum was analyzed by titration of the excess complexone III solution of zinc dichloride [Popova I., Godovannaya I.N. Chelatometric analysis of some dual SP is avow. The journal analytical chemistry. 1965. Volume XX, issue 3. S-356].

The amount of adsorbed metal was determined by difference content in the solution before and after sorption.

E - the degree of extraction of metal from solution, %, was calculated by the formula:

E=(mm/mmex)*100, where

mmex- the mass of the metal in the original solution;

mmthe amount of metal that has fallen into the phase sorbent, ,

The degree of desorption, %, calculated on the basis of the analysis of the solution after elution:

A=(mValente/mm)*100.

BEHOLD - the current value of sorption capacity, mmol/g, found by the formula:

where Mm- the molar mass of the metal, g/mol;

the concentration of metal in the phase sorbent, mg/g, is calculated by the formula:

msat- hanging sorbent,

Below are examples of the implementation of the proposed method of extraction of palladium from spent catalysts for low temperature oxidation of carbon monoxide(II) based on γ-Al2About3containing palladium(II) chloride and copper bromide(II). In the leaching of spent catalysts are formed solutions containing, in addition to palladium chloride and bromide ions. However, preliminary experiments showed that when the molar ratio of CL-:what r -≥50 in the solution as it is implemented in the proposed method, the presence of bromide ions does not influence the efficiency of sorption of palladium.

Example 1. Exhaust catalysts for low temperature oxidation of carbon monoxide(II) based on γ-Al2About3containing palladium(II) chloride and copper bromide(II), were subjected to acid leaching of 1 M Hcl. Extraction of palladium(II) in solution is 94.0±1,0%.

The study of the dependence of the static exchange capacity (SOY) palladium(II) sorbent from the contact time of the phases showed (table 1)that the constant value of the static sorption capacity is achieved for 5-10 minutes stirring phase, while in the prototype, the equilibrium times when sorption is 24 hours a balancing act for palladium(II) for a short time is favorable for carrying out sorption in dynamic mode.

Table 1
The dependence of the sorption capacity of the sorbent for Pd(II) and Cu(II) in static conditions from the time of contact of phases from solution 1 M Hcl (CPDex=1,49 g/l, WithCex=0,89 g/l)
The contact time of the phases, min2510 30456090
COEPd(mg/g3,477,683,278,285,5-73,5
SOYC(mg/g-5,19,08,6-10,4-

Sorption of palladium(II) from 0.1 M Hcl at room temperature were using sorbents, which differ by the number of grafted functional groups: 0.5 mmol/g - Sorbent 1 and 1.63 mmol/g - Sorbent 2. From the presented data shows (table 2)that the best indicators of sorption observed for sorbent containing higher amounts of grafted functional groups, static exchange capacity is 137 mg/g

Table 2
Comparative characteristics of the proposed method and the well-known
PR is lagueny way The known method
The type of sorbentThe sorbent 1Sorbent 2BAU-XLCAO-4LCAO-7
Exchange capacity, mg/g451377,54,52,1
The acidity of solutionspH 1the pH of 1.5

The study of the dependence of the degree of extraction of palladium from acid concentration in the pH range 1-4 M Hcl in static conditions sorbent density prishivki functional groups, part of 1.63 mmol/g, showed that the sorption characteristics of the precious metal ions are observed from solutions with a pH of 1. The data presented in table 3. Preferably, the sorption of lead from solutions with a concentration of Hcl of 0.1-0.5 M

Table 3
The dependence of the sorption capacity of the sorbent for Pd(II) in static conditions on the concentration of Hcl (CPdex=1,49 g/l)
WithHClM0,10,51234
SOY, mg/g13711485727353

Example 2. Sorption of palladium(II) from chloride solutions containing copper(II) and aluminium(III)obtained in example 1. Sorption led from 0.1 M solution of Hcl, the sorbent after sorption were washed with water, palladium was suirable 5%solution of thiourea (Thio) in 0.1 M Hcl. Conducted 2 parallel experience, in the second experiment on the same sorbent spent 3 cycle stages of sorption-desorption to determine the reusability of the sorbent and the stability of its work. In experiment 1 Vex. R-RAis 2.2 ml, experience 2 - 2.0, 1.7, and 1.2 ml, respectively. The solutions obtained in experiment 1, were analyzed by atomic emission method with inductively coupled plasma (table 4). At the stage of sorption of palladium(II) sorbed 99.9%, copper(II) - 15,0-19,0%, aluminum(III) - 1.3-18.8 per cent. At the stage of washing can be almost all copper is removed from the phase sorbent (Σretrieve. Cu in p-p=95-98%), as well as aluminum, that allows to speak about the practice is Cesky full separation of palladium(II) and related metals. Palladium(II) eluted from the sorbent at 85-90%. The proposed sorbent stably withstand more than 3 cycles.

The use of the claimed invention allow for on-stage sorption quantitative extraction of palladium (99,9%) from chloride solutions processing waste palladium catalysts.

EPd, %
Table 4
The results of the experiment on the separation of Pd(II), Cu(II) and Al(III) from hydrochloric acid solution sorbent 1 (CPd=1,60 g/l, WithC=3.11 g/lAl=0.40 g/lHCl=0.1 M)
no experienceSorbentR-R after sorption + PromodeThe eluate 5% Thio in 0.1 M Hcl
mPd, mcgmCu, mcgmAl, mcgEPd, %ECu, %EAl, %Vp-pa,
ml
mCu, mcgWithCu,mcgmlmAl, mcgCAl,mcgmlECu, %EAl, %Vp-pamlmPd, mcgCPd,mcgmlEPd, %
1 experience3520162042099,923,8125258251123100600,0585,496,38312039088,6
2 experience
1 stud.384011134899,915,11,352,47082135379272*-for 95.299,08,5332739190,1
2 stud.272092915399,9of 17.04,651,75146100261751*-98,0to 97.111,4242121289,0
3 stud.19207073609,9 18,317,251,2359170181636*-97,0for 95.29,9162716485,0
*- ions in the solution is not found
Note: the solution of the eluate on Cu(II) and Al(III) were not analyzed

The method of extraction of palladium (II) from spent catalysts include acid leaching of palladium from spent catalysts and sorption of palladium chloride solution, wherein the acid leaching of lead 1 M solution of hydrochloric acid, the resulting solution was diluted with water to a pH of 1 and sorption of palladium carried out on diluted solution of chemically modified silica containing grafted group γ aminopropyltriethoxysilane.



 

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3 cl, 1 tbl, 6 ex

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SUBSTANCE: invention refers to the area of the extraction of gold, palladium and platinum from hydrochloric solutions. The method comprises their anionite sorption and desorption. The sorption shall be performed with low-basic anionites. After sorption, desorption with a mixture of sodium sulfite salts mixture Na2SO3 and sodium nitrite NaNo2.

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