Supported palladium-based catalyst and preparation method and application thereof

A supported palladium and catalyst technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as deactivation, catalytic activity and selectivity decline, and achieve high selectivity.

Active Publication Date: 2016-12-07
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some catalysts that have been reported so far will be deactivated after a period of reaction, and the catalytic activity and selectivity will be seriously reduced.

Method used

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  • Supported palladium-based catalyst and preparation method and application thereof
  • Supported palladium-based catalyst and preparation method and application thereof
  • Supported palladium-based catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Example 1 Preparation of catalyst CAT-1~CAT-16

[0065] Disperse a certain amount of palladium-containing complex into 10 mL of solvent, add dropwise ammonia to adjust the pH of the system to A to obtain system I; add 1 g of carrier and stir and immerse at room temperature for a period of time to obtain system II; heat to the pH of system II It is reduced to B (distilled ammonia), centrifuged, dried, and roasted to obtain a supported palladium-based catalyst sample.

[0066] The relationship between the sample number and the specific preparation conditions is shown in Table 1.

[0067] Table 1

[0068]

[0069]

Embodiment 2

[0070] Example 2 Determination of the content of the components in the catalysts CAT-1~CAT-16

[0071] The element composition of the samples CAT-1 to CAT-16 was measured by Ultima2 inductively coupled plasma emission spectroscopy (ICP) of Jobin Yvon Company. The results are shown in Table 2.

[0072] Table 2

[0073]

[0074]

Embodiment 3

[0075] Example 3 Evaluation of catalytic performance of gas phase carbonylation of methyl nitrite to dimethyl carbonate

[0076] 200 mg of catalysts CAT-1~CAT-16 were respectively put into a fixed-bed tubular reactor, and the reaction evaluation of the gas phase carbonylation of methyl nitrite (abbreviated as MN) to prepare dimethyl carbonate (abbreviated as DMC) was performed respectively. Combine carbon monoxide, methyl nitrite, carrier gas N 2 And internal standard gas Ar (volume ratio CO: MN: Ar: N 2 = 0.17: 0.51: 0.03: 0.29), at a reaction pressure of 0.1 MPa, a reaction temperature of 120 °C, and space velocity = 2500 h -1 The catalysts CAT-1~CAT-12 were contacted respectively under the conditions to obtain the product dimethyl carbonate. The CO conversion rate and DMC selectivity of the catalysts CAT-1~CAT-16 are shown in Table 3.

[0077] The product was detected by Shimadzu's GC-2014 gas chromatograph, 5A and SE-30 columns, TCD and FID dual detectors.

[0078] The conversion...

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PUM

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Abstract

The invention provides a supported palladium-based catalyst and a preparation method and an application thereof. The supported palladium-based catalyst comprises an active ingredient and a carrier, wherein the active ingredient is a palladium-based compound; the carrier is selected from at least one of aluminum oxide, silicon oxide, magnesium oxide, zinc oxide, zirconium oxide, titanium dioxide, metal organic framework compound, activated carbon, molecular sieve, carbon nanotube, and graphene. The supported palladium-based catalyst is applied to the reaction of methyl nitrite vapor-phase carbonylation preparing dimethyl carbonate, and has the advantages that the catalytic activity is high, the product selectivity is high, and the service life is long.

Description

Technical field [0001] The invention belongs to the field of fine chemicals, and specifically relates to a supported palladium-based catalyst and a preparation method and application thereof. Background technique [0002] Dimethyl carbonate is a green and environmentally friendly chemical raw material with a wide range of uses. At present, the methods for synthesizing dimethyl carbonate in industry mainly include phosgene method and transesterification method. The phosgene method is a traditional synthesis method that uses highly toxic phosgene as a raw material, which not only has poor safety, but also pollutes the environment. The by-product HCl is highly corrosive to equipment. The transesterification method uses propylene carbonate and methanol as raw materials for transesterification to produce dimethyl carbonate. The raw material depends on petroleum, and the production cost is high. [0003] The gas-phase carbonylation of methyl nitrite to prepare dimethyl carbonate is a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26B01J31/22B01J31/18B01J31/16B01J31/38C07C68/00C07C69/96
CPCB01J31/16B01J31/1805B01J31/2234B01J31/26B01J31/38B01J2531/824C07C68/00C07C69/96
Inventor 谭洪梓郭国聪徐忠宁陈青松王志巧陈毓敏
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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