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Multicore palladium cluster compound for catalytically hydrolyzing carbon disulfide and carbonyl sulfide

A carbon disulfide, catalytic hydrolysis technology, applied in the preparation/purification of sulfur compounds and sulfur, chemical instruments and methods, etc., can solve the problem of low recovery rate, the catalytic hydrolysis conversion rate of organic sulfides is difficult to reach 100%, and it is difficult to be homogeneous. Catalysis and other problems, to achieve the effect of high-efficiency catalytic cycle process

Active Publication Date: 2016-10-26
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] (2) The active center of organosulfur hydrolysis catalysis and acid gas H 2 The active centers of the catalytic oxidation of S are the same, and it is difficult to greatly increase the catalytic hydrolysis conversion rate of organic sulfides and reach 100% under the conditions of Claus hydrolysis to remove carbon disulfide and carbonyl sulfide.
[0011] (3) In the process of removing carbon disulfide and carbonyl sulfide by Claus dehydration, it is difficult to achieve homogeneous catalysis for the supported catalysts of different particle sizes usually used, and the utilization rate of the catalyst is low and the recovery rate is not high

Method used

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  • Multicore palladium cluster compound for catalytically hydrolyzing carbon disulfide and carbonyl sulfide
  • Multicore palladium cluster compound for catalytically hydrolyzing carbon disulfide and carbonyl sulfide
  • Multicore palladium cluster compound for catalytically hydrolyzing carbon disulfide and carbonyl sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Embodiment 1: the synthesis of (2,2'-bipyridine) palladium nitrate (1a)

[0068] Synthesis of S1(2,2'-bipyridyl)palladium chloride

[0069] 1.0g (5.64mmol) PdCl 2 Dissolve in 150ml of hot acetonitrile at 60°C and add to a 250ml single-necked bottle. Under electromagnetic stirring, 880.9mg (5.64mmol) of 2,2’-bipyridine was dissolved in a small amount of methanol (3mL) and added dropwise to the reaction flask, immediately forming yellow needle-like crystals, which continued to reflux for 2h. Then it was cooled to room temperature, filtered, washed with a small amount of acetonitrile and acetone, and dried to obtain 1.67 g of the product with a yield of 88.3%.

[0070] Synthesis of S2(2,2'-bipyridyl)palladium nitrate

[0071] 1.67g (5.0mmol) bpyPdCl 2 Suspend in 200ml water, add 1.70g (5.0mmol) AgNO dropwise under electromagnetic stirring 3 A small amount of deionized aqueous solution was reacted at 60°C in the dark for 3h. Let stand for 2 hours, filter, and concentr...

Embodiment 2

[0072] Synthesis of Example 2 (4,4'-dimethyl-2,2'-bipyridyl) palladium nitrate (2a)

[0073] Synthesis of S1(4,4'-dimethyl-2,2'-bipyridyl)palladium chloride

[0074] 1.0g (5.64mmol) PdCl 2 Dissolve in 150ml of acetonitrile at 60°C and add to a 250ml single-necked bottle. Under electromagnetic stirring, 5.6 mmol of 4,4'-dimethyl-2,2'-bipyridine was dissolved in a small amount of methanol (3 mL), and added dropwise to the reaction flask, yellow needle-like crystals were formed immediately, and the reflux was continued for 2 h. Then cool to room temperature, filter, wash with a small amount of acetonitrile and acetone, and dry to obtain the product.

[0075] Step S2 is the same as in Embodiment 1. The product is a yellow powder with a yield of 90%.

Embodiment 3

[0076] The synthesis of embodiment 3 (1,10-phenanthroline) palladium nitrate (3a)

[0077] Synthesis of S1(1,10-phenanthroline)palladium chloride

[0078] 1.0g (5.64mmol) PdCl 2 Dissolve in 150ml of acetonitrile at 60°C and add to a 250ml single-necked bottle. Under electromagnetic stirring, 5.5 mmol of 1,10-phenanthroline was dissolved in a small amount of methanol (3 mL), and added dropwise to the reaction flask, yellow needle-like crystals were formed immediately, and the reflux was continued for 2 h. Then cool to room temperature, filter, wash with a small amount of acetonitrile and acetone, and dry to obtain the product.

[0079] Step S2 is the same as in Embodiment 1. The product is a yellow powder with a yield of 91%.

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Abstract

The invention provides a multicore palladium cluster compound for catalytically hydrolyzing carbon disulfide and carbonyl sulfide. The multicore palladium cluster compound is an azacyclo- di-core palladium (II) cluster compound and has the general formula of ([(N^N)2Pd2(NO3)2](NO3)2), wherein (N^N) represents a ligand and is one selected from pyridine, dipyridine, alkylpyridine, pyrroline and phenanthroline. The invention further provides a preparation method for the multicore palladium cluster compound and an application of the multicore palladium cluster compound. The multicore organic-metal cluster compound provided by the invention serves as a catalyst for removing sulfur from the carbon disulfide and the carbonyl sulfide through hydrolysis and is used for catalytically hydrolyzing the carbon disulfide and the carbonyl sulfide in a low-temperature (room-temperature) aqueous solution in a high-efficiency manner so as to produce a carbon dioxide and sulfidion (S<2->) bridged intermediate product of a tri-core palladium cluster compound, and finally, the recycling of the catalyst is achieved through an oxidation-reduction reaction between concentrated nitric acid and the tri-core palladium cluster compound.

Description

technical field [0001] The invention belongs to the field of metal organic compounds, in particular to a metal organic compound containing palladium. Background technique [0002] Carbon disulfide and carbonyl sulfide, as the main sources of air pollutants sulfur dioxide, are converted into sulfur dioxide through light-induced free radical reactions in the atmosphere, causing great harm to air quality, smog and human health. In particular, the content of organic sulfur compounds such as carbon disulfide and carbonyl sulfide in petroleum crude oil exceeds 10%, and the content in crude oil produced in some countries or regions is even higher, and most of the harmful gases are carbonyl sulfide. [1] These chemically inert small organic sulfur molecules have a strong poisonous effect on the metal catalysts used in the petroleum distillation process, and degassing and desulfurization have become an indispensable key step in the petroleum distillation process. [2,3] According to l...

Claims

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Application Information

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IPC IPC(8): C07F15/00B01J31/22C01B17/04
CPCY02P20/584C07F15/0066B01J31/1815B01J31/183C01B17/0404C01B17/0434
Inventor 于澍燕蒋选丰张宁强童金
Owner BEIJING UNIV OF TECH