CS224741B1 - Recovery method of palladium and tin dichloride of waste solutions of colloidal palladium in tin dichloride - Google Patents
Recovery method of palladium and tin dichloride of waste solutions of colloidal palladium in tin dichloride Download PDFInfo
- Publication number
- CS224741B1 CS224741B1 CS394582A CS394582A CS224741B1 CS 224741 B1 CS224741 B1 CS 224741B1 CS 394582 A CS394582 A CS 394582A CS 394582 A CS394582 A CS 394582A CS 224741 B1 CS224741 B1 CS 224741B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- palladium
- tin dichloride
- stannous chloride
- tin
- colloidal
- Prior art date
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims description 68
- 229910052763 palladium Inorganic materials 0.000 title claims description 34
- 229910021626 Tin(II) chloride Inorganic materials 0.000 title claims description 22
- 235000011150 stannous chloride Nutrition 0.000 title claims description 22
- 238000000034 method Methods 0.000 title claims description 15
- 239000002699 waste material Substances 0.000 title claims description 6
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 title description 4
- 238000011084 recovery Methods 0.000 title description 3
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 18
- 239000001119 stannous chloride Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 11
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- -1 nitrate ions Chemical class 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- AZEGRRQOQSUJJK-UHFFFAOYSA-N nitrate;hydrochloride Chemical compound Cl.[O-][N+]([O-])=O AZEGRRQOQSUJJK-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Description
(54) Způsob získávání palladia a chloridu cínatého z odpadních roztoků kcloidního palladia v chloridu cínatém(54) A method for recovering palladium and stannous chloride from cloloid palladium waste solutions in stannous chloride
Vynález se týká způsobu získávání palladia a roztoku chloridu cínatého z odpadních i aktivačních lázní pro bezproudé pokovování nekovových povrchů, jejichž podstatou je kloidni. roztok palladia v chloridu cínatém. Týto aktivační lázně mohou dále obsahoval různé dalěí anorganické i organické látkyPro získávání palladia z těchto roztoků byl publikován jen jediný postup. Podle popisu vynálezu k maďarskému patentu č. 11100 ja palladium z roztoků získáváno přídavkem koncentrované kyseliny dusičné. Nevýhodou postupu je znečištění roztoku chloridu cínatého ionty dusičnanovými a postup se hodí pouze pro obsahy palladia v roztocích nad 0,4 g pslladia/dm^. Tento poatup však neřeší získávání chloridu cínatého vedle palladia, který je v tomto případě znečištěn dusičnanovými ionty, tudíž je odpadem nebo produktem a omezeným využitím.The present invention relates to a process for obtaining palladium and a stannous chloride solution from waste and activation baths for electroless plating of non-metallic surfaces based on cloid. solution of palladium in stannous chloride. The activation bath may further contain various other inorganic and organic substances. Only one procedure has been published for recovering palladium from these solutions. According to the description of the invention to Hungarian patent No. 11100, palladium is obtained from the solutions by the addition of concentrated nitric acid. The disadvantage of the process is that the nitrate chloride solution is contaminated with nitrate ions and the process is only suitable for palladium contents in solutions above 0.4 g psl / dm @ 2. However, this approach does not address the recovery of stannous chloride in addition to palladium, which in this case is contaminated with nitrate ions, thus being a waste or product and a limited recovery.
. Uvedené nevýhody podstatně snižuje způsob získávání palladia a chloridu cínatého z odpadních roztoků koloidního palladia v chloridu cínatém podle vynálezu, který počívá v tom, že ae do koloidního roztoku palladia v chloridu cínatém přidává kov. S výhodou se dále do roztoku přidává kyselina chlorovodíková, případně cín.. These disadvantages are substantially reduced by the method of recovering palladium and stannous chloride from the waste solutions of colloidal palladium in stannous chloride according to the invention, which comprises adding metal to the colloidal palladium in stannous chloride solution. Preferably, hydrochloric acid or tin is further added to the solution.
Způsob získávání palladia a chloridu cínatého z koloidních roztoků palladia v chlori_ du cínatém je výhodný tím, že je založen na koagulaci koloidního roztoku kovy, uvolňující z kyseliny chlorovodíkové vodík. Při koagulaci koloidního roztoku palladia v chloridu cína224741 tém cínem se do roztoku nezanáší delší lonty. Koagulace je urychlována zvýšením teploty, zvýšením koncentrace vodíkových iontů a zvýšením měrného povrchu kovu.The process for obtaining palladium and stannous chloride from colloidal solutions of palladium in stannous chloride is advantageous in that it is based on the coagulation of the colloidal solution with metals releasing hydrogen from the hydrochloric acid. When coagulating a colloidal palladium solution in tin chloride with tin, no longer ions are introduced into the solution. Coagulation is accelerated by increasing the temperature, increasing the concentration of hydrogen ions, and increasing the specific surface of the metal.
Tímto postupem se získá palladium ve výtěžku 99,9 % ve formě surového kovu a současně roztok chloridu cínatého, který se hodí k průmyslovému použití. Kosgulované palladium tímto postupem obsahuje sice značné množství nečistot, ale obvyklými rafinačními postupy lze dospět k čistému palladiu a jeho sloučeninám.This gives palladium in a yield of 99.9% in the form of a crude metal and at the same time a solution of stannous chloride which is suitable for industrial use. While this process contains a significant amount of impurities in this process, it is possible to obtain pure palladium and its compounds by conventional refining processes.
Účinek způsobu podle vynálezu spočívá v tom, že umožňuje získávání palladia z koloidních roztoků palladia v chloridu cínatém v širokém koncentračním rozmezí obou uvažovaných kovů téměř kvatitativně.The effect of the process according to the invention is that it makes it possible to obtain palladium from colloidal solutions of palladium in tin (II) chloride in a wide concentration range of the two metals under consideration almost quantitatively.
Příklad 1Example 1
K 0,5 dm^ roztoku obsahujícího 0,24 g palladia/dm^ a 43,77 g cínu/dm^ a 38,3 g kyseliny chlorovodíkové/dm^ bylo přidáno 15,0 g kovového cínu ve formě hoblin. Reakční směs byla zahřívána na teplotu 90 °C a míchána 2 h. Pak ae nechalo kosgulované palladium usadit, čirý roztok chloridu cínatého byl odlit a palladium bylo dekantováno třikrát po 0,1 dm^ destilované vody. Po dekantaci bylo sušeno 2 h při 140 °C. Získalo se tak 0,475 dm-} roztoku chloridu cínatého s obsahem 77,63 g cínu/dm^ a 0,2153 g palladia s obsahem 55,73 % palladia.To 0.5 dm 2 of a solution containing 0.24 g of palladium / dm 2 and 43.77 g of tin / dm 2 and 38.3 g of hydrochloric acid / dm 2 was added 15.0 g of metal tin as shavings. The reaction mixture was heated to 90 ° C and stirred for 2 h. After allowing the clogged palladium to settle, the clear stannous chloride solution was discarded and the palladium was decanted three times with 0.1 dm 3 of distilled water. After decantation, it was dried at 140 ° C for 2 h. There was thus obtained a 0.475 dm - solution of tin (II) chloride containing 77.63 g of tin / dm 2 and 0.2153 g of palladium with 55.73% palladium.
Příklad 2Example 2
K 0,3 dm^ roztoku obsahujícímu 3,0 g palledia/dm^, 187,5 g cínu/dm^ a 72,3 g kyselinyTo a 0.3 dm ^ solution containing 3.0 g palladium / dm ^, 187.5 g tin / dm ^ and 72.3 g of acid
3 chlorovodíkové/dm bylo přidáno 50,0 g práškového cínu a 0,15 dmJ 35 % kyseliny chlorovodíkové. Reakční směs byle zpracována jako v příkladu 1 a bylo získáno. 0,9889 g palladia s obsahem 91,0 % palladia a 0,432 dm^ roztoku obsahujícího 245,1 g cínu/dnA3 HCl / dm was added 50.0 g tin powder and 0.15 dm J 35% hydrochloric acid. The reaction mixture was worked up as in Example 1 and was obtained. 0.9889 g of palladium containing 91.0% palladium and 0.432 dm @ 2 of a solution containing 245.1 g of tin / dnA
V obou případech roztoky chloridu cínatého neobsahovaly ani stopy palladia·'In both cases, the stannous chloride solutions contained no traces of palladium.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS394582A CS224741B1 (en) | 1982-05-28 | 1982-05-28 | Recovery method of palladium and tin dichloride of waste solutions of colloidal palladium in tin dichloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS394582A CS224741B1 (en) | 1982-05-28 | 1982-05-28 | Recovery method of palladium and tin dichloride of waste solutions of colloidal palladium in tin dichloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS224741B1 true CS224741B1 (en) | 1984-01-16 |
Family
ID=5381004
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS394582A CS224741B1 (en) | 1982-05-28 | 1982-05-28 | Recovery method of palladium and tin dichloride of waste solutions of colloidal palladium in tin dichloride |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS224741B1 (en) |
-
1982
- 1982-05-28 CS CS394582A patent/CS224741B1/en unknown
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