Method for reclaiming metal palladium and palladium chloride from waste loading palladium hydrogenation catalyst

A technology of hydrogenation catalyst and metal palladium, which is applied in the direction of improving process efficiency, etc., can solve the problems of incompletely applicable treatment, and achieve the effects of avoiding equipment investment and operating costs, flexible process, low equipment investment and operating costs

Inactive Publication Date: 2009-09-09
XIAMEN KINGDOMWAY VI TAMIN INC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above method is not fully applicable to the treatment of Lindela catalyst
There are also environmental protection problems with aqua regia treatment, so it should not be used as much as possible.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The composition of the spent Lindella catalyst generally contains 1% to 10% palladium, 1% to 10% Pb, Bi, Fe, Mg, Hg, Sn, Zn and other metal salts, 1% to 10% organic impurities , and the rest are carriers, mainly carbonates (such as CaCO 3 ).

[0041] Weigh 20g of the spent Lindra catalyst containing 3.5% palladium, add 100ml of 95% ethanol and 2g NaOH to reflux for 1h, wash the organic matter and decompose the carrier with 100ml of 20% hydrochloric acid, and then disperse the obtained crude palladium with 10ml of 35% hydrochloric acid. Add 2ml of 30% hydrogen peroxide, oxidize and dissolve palladium at 20-90°C, add ammonia water with a concentration of 30% to the solution until pH = 9, filter and remove the filter cake to obtain palladium-ammonia solution, and add palladium ammonia solution at 40-100°C Add 1ml of 80% hydrazine hydrate to the ammonia solution, and a black spongy palladium precipitate will form. Filter it, wash it with hot deionized water and drain it 30...

Embodiment 2

[0043] Change the step of "adding 100ml 95% ethanol and 2g NaOH to reflux for 1h" in Example 1 to: add 100ml chloroform and 0.1g surfactant fatty alcohol polyoxyethylene ether (AOE), and put it into ultrasonic treatment for 1h. The rest of the steps are the same with the same result.

Embodiment 3

[0045] Change the step of "adding 100ml 95% ethanol and 2g NaOH to reflux for 1h" in Example 1 to: add 200ml petroleum ether and 0.1g surfactant alkylphenol polyoxyethylene ether (APEO), heat and stir to reflux for 1h. The rest of the steps are the same with the same result.

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PUM

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Abstract

A method to recover Pd and Palladium Chloride from waste Pd loading hydrogenation activator, the patent provides a method to reclaim Pd and Palladium Chloride with high purity from waste activator, especially form Lindla activator. The organic substance impurity adhere to the surface of the waste Pd loading hydrogenation activator will be get rid by solution, the activator, which has been treated, will be added acid to decompose and get rid of the carbonate in the carrier, and the raw Pd will be gained. The raw Pd will be oxidized and dissolved to produce chorosub-palladium acid by hydrochloric acid-double oxygen water, and Pd solution can be gained. Ammonia will be added into the Pd solution to aminate, and the inorganic impurity such as Pb and Bi will be filtrated and get rid as deposit. Reducing agent will be used to deoxidize and deposit the cavernous Pd with high purity from Palladium-ammonia solution. The cavernous Pd will be oxidized and dissolved with hydrochloric acid-double oxygen water, and then will be evaporated to dryness to produce palladium chloride with high purity.

Description

technical field [0001] The invention relates to a method for recovering high-purity metallic palladium and palladium chloride from spent supported palladium hydrogenation catalysts, especially spent Lindella catalysts. Background technique [0002] Lindra catalyst is a unique supported palladium hydrogenation catalyst. Lindlar (H.Lindlar) of Roche Company (Hoffman.La Roche Inc.) discloses a kind of loading in CaCO for the first time in US Pat. 3 Preparation method of catalyst modified with lead salt, or bismuth salt, or lead-bismuth mixture on carrier and application of the catalyst to vitamin A intermediate, 1,6-dihydroxy-3,7-dimethyl-9-( Hydrogenation of 2', 6', 6'-trimethyl-1'-cyclohexene)-2,7-nonadiene-4-yne. The catalyst selectively hydrogenates only the acetylenic bonds of the above-mentioned intermediates, and only hydrogenates to the olefinic bonds, and the multi-ene bonds originally present in this compound are basically not affected. The highly selective hydroge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B11/00C22B3/04C22B3/22C22B3/44C22B7/00
CPCY02P10/20
Inventor 付志杰陈德安魏初权刘华英
Owner XIAMEN KINGDOMWAY VI TAMIN INC
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