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Water-soluble pt(iv) complex and its preparation method and use

A complex and water-soluble technology, applied in platinum-based organic compounds, chemical instruments and methods, platinum-group organic compounds, etc., can solve the problems of unsuitable catalyst preparation and low water solubility of precursor compounds

Active Publication Date: 2022-07-08
KUNMING INST OF PRECIOUS METALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese patent CN 101255176 A discloses a new type of platinum Pt(II) precursor compound [Pt(NH 3 ) 4 ]X 2 (X 2 organic carboxylic acid), although this type of precursor compound itself does not contain chloride ion and nitrate, but the water solubility of this type of catalytic precursor compound is low (room temperature is less than 20mg / ml), it is not suitable for the preparation of some high platinum loading amount of catalyst

Method used

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  • Water-soluble pt(iv) complex and its preparation method and use
  • Water-soluble pt(iv) complex and its preparation method and use
  • Water-soluble pt(iv) complex and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: Intermediate trans-[Pt(NH 3 ) 4 (OH) 2 ](HCO 3 ) 2 preparation

[0036] Weigh 80 g (207 mmol) [Pt (NH 3 ) 4 ](NO 3 ) 2 , dissolve in 800mL of water, add 125ml (1115mmol) of 30% hydrogen peroxide solution, heat under reflux for reaction, and gradually precipitate out white trans-[Pt(NH 3 ) 4 (OH) 2 ](NO 3 ) 2 Precipitate, after 8 hours, at 60 ℃ under alkaline pressure to concentrate to 100mL, filter and collect, after washing twice with a small amount of water, transfer to a 1500mL reaction flask, add 200mL of water, stir into slurry, add dropwise while stirring 800 mL of ammonium bicarbonate aqueous solution (containing 150 g of ammonium bicarbonate, equivalent to 1900 mmol), continue to stir and react at 50 ° C for 24 hours, then concentrate under reduced pressure at 50 ° C to 200 mL, and filter to collect the precipitated product trans-[Pt (NH 3 ) 4 (OH) 2 ](HCO 3 ) 2 , washed 3 times with a small amount of water to remove residual nitrate...

Embodiment 2

[0037] Example 2: trans-[Pt(NH 3 ) 4 (OH) 2 ](CH 3 COO) 2 ·2H 2 Synthesis of O

[0038] Measure 10 mL (173 mmol) of 99% acetic acid, dilute it to 50 mL with water, and slowly add it dropwise to 30 g of trans-[Pt(NH) under the greenhouse. 3 ) 4 (OH) 2 ](HCO 3 ) 2 (72mmol), stir while adding dropwise, the intermediate dissolves and emits CO2 gas, after the dropwise addition, heat at 50°C for 45min to form a colorless and clear solution, after cooling, filter to remove trace insolubles, the filtrate is at 50°C It was concentrated to near dryness under reduced pressure to obtain a white crystalline powder, which was dried at 50 °C for 2 hours to obtain 32 g of trans-[Pt(NH 3 ) 4 (OH) 2 ](CH 3 COO) 2 ·2H 2 O, 98.8% yield

[0039] Structural characteristic parameters: Elemental analysis: measured values ​​Pt 43.0%, C 10.5%, H 5.39%, N 12.2% (calculated values ​​Pt 43.2%, C 10.6%, H 5.32%, N 12.4%); IR(cm -1 ,KBr): 3225(s,v(NH 3 )), 1541(s,v as (COO - )), 1410(...

Embodiment 3

[0040] Example 3: [Pt(NH 3 ) 5 (OH)](CH 3 COO) 3 Synthesis

[0041] Weigh 40 g of trans-[Pt(NH 3 ) 4 (OH) 2 ](HCO 3 ) 2 (96mmol) in a reaction flask, add 25-28% ammonia water 150mL (2290mmol), stir the reaction at 55°C for 10 hours, and concentrate under reduced pressure to 50mL at 55°C, collect the product by filtration, and wash 3 times with a small amount of water to remove unreacted ammonia, followed by vacuum drying at 55 °C for 4 h, yielding 36 g of [Pt(NH 3 ) 5 (OH)] 2 (CO 3 ) 3 , the yield is 97%. The measured value of platinum content is 50.1%, which is consistent with the theoretical value of 50.4%.

[0042] Measure 16 mL (277 mmol) of 99% vinegar, dilute it with water to 80 mL, and slowly add it dropwise to 30 g of [Pt(NH) under the greenhouse. 3 ) 5 (OH)] 2 (CO 3 ) 3 (39mmol), stir while adding dropwise, the reactant dissolves and emits CO2 gas, after the dropwise addition, it is heated at 50 ° C for 45 min to form a colorless and clear solution,...

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Abstract

The present invention relates to two Pt(IV) complexes trans-[Pt(NH 3 ) 4 (OH) 2 ]X 2 , [Pt(NH 3 ) 5 (OH)]X 3 (X=CH 3 COO ‑ ) and their preparation method and use, wherein, with ammonia and OH — It is an internal ligand, which forms a 6-coordinated octahedral cation with Pt(IV), and X is an external anion, which has a charge balance effect. Their synthesis is based on commercially available Pt(II) compounds [Pt(NH 3 ) 4 ](NO 3 ) 2 As the starting material, the product is obtained through chemical reactions such as axial oxidation, external exchange, internal coordination substitution, and external neutralization. The synthesis conditions of the invention are mild, easy to control, and the yield is high, and batch synthesis can be realized. The two Pt(IV) complexes do not contain chlorine, nitrate and other elements and components that are harmful to the catalyst, have high water solubility, and have low thermal decomposition temperature. The supported platinum catalyst prepared as a catalytic precursor has good performance. , which can be used for industrial production of supported platinum catalysts.

Description

technical field [0001] The invention relates to two water-soluble Pt(IV) complexes, a preparation method and application thereof, in particular to two water-soluble Pt(IV) complexes free of chlorine and nitrate, a chemical synthesis method and a method for preparing a supported platinum catalyst applications in . Background technique [0002] Supported platinum catalyst is an important heterogeneous reaction catalyst, which is widely used in various fields such as petrochemical, pharmaceutical and fine chemical, new energy, industrial harmful waste gas and automobile exhaust purification, etc. At present, the mainstream method for preparing supported platinum catalysts is chemical impregnation method. China Materials Engineering Encyclopedia. Volume 5, 504-594, Chemical Industry Press, 2006], liquid phase loading is one of the key steps. Liquid phase loading involves the selection and use of catalytic precursors. The catalytic precursor is a soluble platinum compound, whi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00B01J23/63B01J37/02B01J37/08
CPCC07F15/0093B01J23/63B01J37/0201B01J37/08Y02P20/584
Inventor 刘伟平余娟李雪高安丽姜婧陈力常桥稳晏彩先张振强
Owner KUNMING INST OF PRECIOUS METALS
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