Water soluble Pt(II) catalyst precursor free from chlorine and nitrate and synthetic method thereof

A technology of nitrate and precursor, applied in the field of precursor compounds, can solve the problem of low water solubility

Inactive Publication Date: 2013-05-22
KUNMING INST OF PRECIOUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these catalytic precursor compounds have low water solubility (less than 20mg / ml at room temperature), and are not suitable for the preparation of some highly loaded platinum catalysts. It is necessary to find similar compounds with high water solubility

Method used

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  • Water soluble Pt(II) catalyst precursor free from chlorine and nitrate and synthetic method thereof
  • Water soluble Pt(II) catalyst precursor free from chlorine and nitrate and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1, the synthesis of tetraammine platinum acetate (II)

[0013] Weigh 3.52 g (10 mmol) [Pt(NH 3 ) 4 ] Cl 2 ·H 2 Dissolve O in 50 mL of water, add 3.34 g (20 mmol) of silver acetate solid in batches under stirring, stir and react for 2 hours after the addition is complete, let stand, filter, wash the filter residue with 50 mL of water for 3 times, and combine the filtrate and washing liquid After concentrating to about 5 mL, add 50 mL of ethanol, stir for 15 minutes, let stand for 30 minutes, collect by filtration, and dry at 110°C for 2 hours to obtain 3.63 g of [Pt(NH 3 ) 4 ](CH 3 COO) 2 Product, yield 95.2%.

[0014] Structural characteristic parameters: Elemental analysis: measured values ​​C 12.53%, H 4.81%, N 14.65%, Pt 51.02% are consistent with theoretical values ​​C 12.60%, H 4.76%, N 14.69%, Pt 51.16%. IR (cm -1 , KBr) 3261, 3221 (s, ν(NH 3 )); 1696, 1652 (s, ν as (C=O)), 1405 (s, ν s (C=O)). 1 H NMR (D 2 O, ppm) 1.76 (s, 3H, CH 3 ...

Embodiment 2

[0015] Embodiment 2, the synthesis of tetraammine platinum acetate (II)

[0016] Take by weighing 333.8 grams of silver acetate, add 200 mL of water and stir it into a paste, then slowly add the paste to 352.0 grams of [Pt(NH 3 ) 4 ] Cl 2 ·H 2 Dissolve O in a solution of 3 L of water, stir for 3 hours, let stand, filter, wash the filter residue with 2 L of water for 3 times, combine the filtrate and washing liquid and concentrate to about 200 mL, add 2 L of ethanol, and stir for 30 minutes Let stand for 30 minutes, collect by filtration, and dry at 80° C. for 2 hours to obtain 385.0 grams of [Pt(NH 3 ) 4 ](CH 3 COO) 2 ·H 2 O product, yield 96.4%.

[0017] Structural characteristic parameters: Elemental analysis: measured values ​​C 11.85%, H 5.03%, N 14.05%, Pt 48.82% are consistent with theoretical values ​​C 12.03%, H 5.05%, N 14.03%, Pt 48.85%. IR (cm -1 , KBr) 3403 (s, ν(H 2 O)); 3261, 3221 (s, ν(NH 3 )); 1696, 1652 (s, ν as (C=O)), 1405 (s, ν s (C=O)). ...

Embodiment 3

[0018] Example 3, Preparing Pt / Al with Tetraammine Platinum (II) Acetate as a Precursor 2 o 3 catalyst

[0019] Immerse the alumina carrier in 30 ml of 0.05 mol / L tetraammine platinum acetate solution, soak for 5 hours at room temperature, drain, dry at 120°C for 4 hours, and then bake at 500°C for 4 hours to obtain a content of 0.3 %Pt / Al 2 o 3 Catalyst Pt1 of the catalyst; chloroplatinic acid and platinum nitrate solutions were used as precursors to prepare Pt / Al with a content of 0.3% by the same method as above 2 o 3 Catalysts Pt2 and Pt3.

[0020] Taking the hydrogenation of benzene to cyclohexane as a reaction model to investigate their catalytic activity, the reaction conditions are: a mixture of hydrogen and benzene (2000: 1) was introduced at 170°C and 3 MPa. The reaction results of the above catalysts are shown in the following table:

[0021]

[0022] It can be seen from the above table that the performance of the catalyst for the hydrogenation of benzene t...

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Abstract

The invention relates to a water soluble Pt(II) catalyst precursor free from chlorine and nitrate and a synthetic method thereof. The invention discloses a precursor compound: tetraammineplatinumdiacetate for preparing a supported platinum catalyst, wherein the molecular formula is [Pt(NH3)4](CH3COO)2.nH2O, n=0, 1. The compound is prepared by the step of performing reaction of tetraammineplatinum chloride hydrate as a starting raw material and silver acetate to obtain the target compound tetraammineplatinumdiacetate. The yield is greater than 95%. The compound as the precursor has the characteristics that (1) the compound is free from elements such as chlorine, sulphur and phosphorus harmful to catalysis; (2) the compound is quite high in water solubility and can be used as a the precursor of the highly supported platinum catalyst with the solubility in water reaching 80g / 100g; (3) the compound in aqueous liquor is dissociated to release stable complex cations [Pt(NH3)4]2+ to the benefit of absorbing the precursor compound by a carrier in impregnation; and (4) own redox reaction of the compound occurs at 300 DEG C to directly generate platinum without gases harmful to the environment. The precursor is an ideal precursor for the supported catalyst by an impregnation method.

Description

technical field [0001] The invention relates to a precursor compound for preparing a supported platinum catalyst—tetraammine platinum acetate and a synthesis method thereof, belonging to the field of chemical catalysis. Background technique [0002] Supported platinum catalysts are an important class of heterogeneous reaction catalysts, which are widely used in various fields such as petrochemical, pharmaceutical and chemical, automobile exhaust and environmental treatment. At present, the main method of preparing platinum-supported catalysts is the impregnation method, that is, the carrier (such as activated alumina, silica, activated carbon, etc.) is soaked in the impregnation solution containing platinum precursor compounds, then drained, dried, and finally roasted and passed through hydrogen. Reductive activation to obtain a supported platinum catalyst for industrial applications. Currently commonly used platinum precursor compounds are mainly chlorides (such as chlorop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00B01J23/42
Inventor 叶青松刘伟平陈家林余娟常桥稳姜婧晏彩先
Owner KUNMING INST OF PRECIOUS METALS
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