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Method for separating enriched palladium by adopting supermolecule secondary spherical coordination identification

A separation, enrichment and supramolecular technology, applied in the field of extracting metal palladium, can solve the problems of consuming oxidants and reducing agents, and achieve the effect of broad industrial application prospects.

Inactive Publication Date: 2009-09-09
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ammonium chloropalladate precipitation method uses repeated oxidation-reduction to remove base metals, consuming large amounts of oxidizing and reducing agents

Method used

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  • Method for separating enriched palladium by adopting supermolecule secondary spherical coordination identification
  • Method for separating enriched palladium by adopting supermolecule secondary spherical coordination identification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Preparation of protonated dibenzylamine

[0019] Take 5g of dibenzylamine, add 10ml of chloroform, after dissolving, add 0.5ml of 37% hydrochloric acid, a white precipitate is formed, filter and dry in vacuo.

[0020] (2) Preparation of palladium-containing sample solution

[0021] PdCl 2 0.0201g, AlCl 3 0.0153g, FeCl 3 ·6H 2 O 0.0316g, NiCl 2 ·6H 2 O 0.0256g, CoCl 2 ·6H 2 O 0.0269g, CuCl 2 2H 2 O 0.0185g, MnCl 2 4H 2 O 0.0229g, add to 150mL beaker, add 10ml of water and 1ml of concentrated hydrochloric acid, dissolve.

[0022] (3) Separation and enrichment of palladium:

[0023] Add protonated dibenzylamine methanol solution (protonated dibenzylamine 0.15g, dissolved in 20ml methanol) to the palladium-containing sample solution prepared above, add 1ml 20% hydrochloric acid, let stand for 20 hours, and precipitate reddish-brown crystals. After filtration, the obtained solid was vacuum-dried to obtain complex powder, and the recovery rate of palladium...

Embodiment 2

[0034] (1) Preparation of protonated dibenzylamine

[0035] Take 5g of dibenzylamine, add 10ml of chloroform, after dissolving, add 0.5ml of 37% hydrochloric acid, a white precipitate is formed, filter and dry in vacuo.

[0036] (2) Preparation of palladium-containing sample solution

[0037] As shown in Table 2, weigh PdCl 2 and AlCl 3 In a 150mL beaker, add 5ml of water and 0.5ml of hydrochloric acid.

[0038] (3) Separation and enrichment of palladium:

[0039] Add an ethanol solution of protonated dibenzylamine to the palladium-containing sample solution prepared above (0.1 g of protonated dibenzylamine is dissolved in 20 ml of ethanol), add 1 ml of 10% sulfuric acid, and let it stand for 15 hours to obtain a reddish-brown solution, and a reddish-brown solution is precipitated. brown crystals. Filter and dry in vacuo to obtain complex powder.

[0040] Take 0.1975g of the dried complex powder, add 10ml of ammonia water, stir in a closed container for 50min until the r...

Embodiment 3

[0046] (1) Preparation of protonated dibenzylamine

[0047] Take 5g of dibenzylamine, add 10ml of chloroform, after dissolving, add 0.5ml of 37% hydrochloric acid, a white precipitate is formed, filter and dry in vacuo.

[0048] (2) Preparation of palladium-containing sample solution

[0049] As shown in Table 3, weigh PdCl 2 and FeCl 3 ·6H 2 O was dissolved in a 150mL beaker by adding 5ml of water and 0.5ml of hydrochloric acid.

[0050] (3) Separation and enrichment of palladium:

[0051] Add protonated dibenzylamine tert-butanol solution (protonated dibenzylamine 0.10g, dissolve in 20ml tert-butanol) to the palladium-containing sample solution prepared above, add 1ml 12% nitric acid, and let it stand for 24 hours to obtain Reddish-brown solution, reddish-brown crystals were precipitated. Filter and dry in vacuo to obtain complex powder.

[0052] Take 0.2012g of the dried complex powder, add 10ml of ammonia water, stir in a closed container for 50min until the reddish...

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Abstract

The invention relates to a method for separating enriched palladium by adopting supermolecule secondary spherical coordination identification. The method adopts the technical scheme as follows: taking a certain amount of sample solution containing palladium, adding an alcoholic solution of protonized dibenzyl amine to the sample solution containing palladium, adding acid to the mixture, standing the new mixture for 5 hours to 24 hours, filtering the new mixture to obtain solid complexes, drying the obtained solid complexes, dissolving the obtained solid complexes with ammonia, extracting the obtained solid complexes with inert organic solvent to separate organic phases; and taking a water phase as a solution for extracting the palladium, wherein the alcoholic solution can be ethanol, tert-butyl alcohol, n-propanol, isopropyl alcohol, carbinol, n-butyl alcohol, isobutyl alcohol or glycol, the acid can be hydrochloric acid, sulphuric acid, nitric acid, acetic acid, p-toluene sulfonic acid, benzene sulfonic acid and trifluoroacetic acid or the mixture of some of the same, and the inert organic solvent can be nitrobenzene, bromobenzene, chlorobenzene, petroleum ether, chloroform, paraffinic oil, coal oil, methylene dichloride, benzene, toluene or dimethylbenzene or the mixture of some of the same. With the method, the palladium can be rapidly separated from other base metals with high efficiency and high selectivity.

Description

technical field [0001] The invention relates to a method for extracting metal palladium. In particular, it relates to a method of using supramolecular crystal engineering and the basic principle of secondary spherical coordination to realize the selective separation and enrichment of precious metal palladium by protonating dibenzylamine with a simple and easy-to-obtain second ligand. Background technique [0002] Metal palladium (Pd) has excellent chemical corrosion resistance, excellent high temperature performance, high chemical activity and stable electrical characteristics, so it is widely used in cutting-edge science and modern industries such as petrochemical, electronic and electrical, environmental protection, biopharmaceutical, and national defense. play a key and central role. Because palladium resources are very limited (the content in the earth's crust is scarce and the distribution is very uneven), thus recovering metal palladium from spent palladium catalysts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B11/00C22B7/00C07C209/68C07C211/27
CPCY02P10/20
Inventor 郭放宋纯亮郭文生
Owner LIAONING UNIVERSITY
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