Supported palladium catalyst as well as preparation method and application thereof

A supported palladium and catalyst technology, applied in the field of Pd catalyst and its preparation, can solve the problems of limiting the hydrogenation rate of alkylanthraquinone derivatives, the yield of hydrogen peroxide, low activity and the like

Pending Publication Date: 2021-09-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In contrast, the silica-supported Pd catalyst has high selectivity and less degradation products, but its activity

Method used

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  • Supported palladium catalyst as well as preparation method and application thereof
  • Supported palladium catalyst as well as preparation method and application thereof
  • Supported palladium catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Dissolve 2.4g of triblock polymer P123 in 90mL of 1.30M HCl solution at 40°C, and then slowly add 4.25g of tetraethyl orthosilicate (TEOS) to obtain a reaction solution with a molar composition of P123:TEOS=1:49. The reaction solution was stirred at 40°C for 24h, then transferred to an autoclave and heated at 100°C for 48h. The reaction solution was filtered, and the obtained solid was washed three times with distilled water, filtered, dried at 110° C. for 12 hours, and then calcined at 550° C. in an argon atmosphere for 6 hours to obtain a mesoporous silica molecular sieve carrier modified with pore wall carbon membrane. The obtained support was impregnated with palladium in an equal volume, calcined in an argon atmosphere at 550°C for 4 hours, and reduced in an atmosphere of 10% hydrogen / 90% argon (volume %) at 250°C for 2 hours to prepare a supported palladium catalyst, which was designated as PD3550. The carbon content and properties of the catalyst supports are sho...

Embodiment 2

[0043] Dissolve 2.4g of triblock polymer P123 in 90mL of 1.30M HCl solution at 40°C, and then slowly add 4.25g of tetraethyl orthosilicate (TEOS) to obtain a reaction solution with a molar composition of P123:TEOS=1:49. The reaction solution was stirred at 40°C for 24h, then transferred to an autoclave and heated at 100°C for 48h. The reaction liquid was filtered, and the obtained solid was washed three times with distilled water, filtered, dried at 110° C. for 12 hours, and then calcined at 650° C. in an argon atmosphere for 6 hours to obtain a mesoporous silica molecular sieve carrier modified with pore wall carbon membrane. The obtained carrier was impregnated with palladium in an equal volume, calcined in an argon atmosphere at 550°C for 4h, and reduced in an atmosphere of 10% hydrogen / 90%argon (volume %) at 250°C for 2h to prepare a supported palladium catalyst, which was designated as PD3650. The carbon content and properties of the catalyst supports are shown in Table 1...

Embodiment 3

[0046] Dissolve 2.4g of triblock polymer P123 in 90mL of 1.30M HCl solution at 40°C, and then slowly add 4.25g of tetraethyl orthosilicate (TEOS) to obtain a reaction solution with a molar composition of P123:TEOS=1:49. The reaction solution was stirred at 40°C for 24h, then transferred to an autoclave and heated at 100°C for 48h. The reaction liquid was filtered, and the obtained solid was washed three times with distilled water, filtered, dried at 110° C. for 12 hours, and then calcined at 750° C. in an argon atmosphere for 6 hours to obtain a mesoporous silica molecular sieve carrier modified with pore wall carbon membrane. The obtained support was impregnated with palladium in an equal volume, calcined in an argon atmosphere at 550°C for 4h, and reduced in an atmosphere of 10% hydrogen / 90% argon (volume %) at 250°C for 2h to prepare a supported palladium catalyst, which was designated as PD3750. The carbon content and properties of the catalyst supports are shown in Table ...

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Abstract

The invention discloses a supported palladium catalyst as well as a preparation method and application thereof. The supported palladium catalyst comprises a mesoporous silica molecular sieve carrier modified by a pore wall carbon membrane, and active metal palladium, the content of carbon in the mesoporous silica molecular sieve carrier is 0.5-3.5 wt%, and the contact angle of the mesoporous silica molecular sieve carrier is 20-60 degrees. The catalyst is used for anthraquinone derivative hydrogenation, has hydrophobicity and good long-range orderliness, obviously improves the alkyl anthraquinone derivative hydrogenation rate and the hydrogen peroxide yield, and reduces the degradation product yield. In addition, the preparation method disclosed by the invention has the advantages of simplicity and high efficiency.

Description

technical field [0001] The invention relates to a Pd catalyst, a preparation method thereof, and an application of the Pd catalyst in the hydrogenation of anthraquinone derivatives. Background technique [0002] Hydrogen peroxide (H 2 o 2 ) is a very widely used green chemical, which has continued to grow rapidly over the years. With the successful development and industrial application of the process of direct liquid phase oxidation of propylene to propylene oxide (HPPO process) and the process of producing ε-caprolactam by ammonia oxidation of cyclohexanone, while the demand for hydrogen peroxide has increased significantly, its quality (concentration and purity) also put forward higher requirements. [0003] At present, the anthraquinone method is still the mainstream technology for the production of hydrogen peroxide. The anthraquinone method includes four main processes of hydrogenation, oxidation, extraction and regeneration. Under the action of the catalyst, the ...

Claims

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Application Information

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IPC IPC(8): B01J29/03B01J37/02B01J37/06B01J37/08C01B15/023
CPCB01J29/0325B01J29/0308B01J37/08B01J37/084B01J37/06B01J37/0207C01B15/023B01J2229/18
Inventor 徐伟张帆王楠贾学五石宁
Owner CHINA PETROLEUM & CHEM CORP
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