Activated carbon-supported nitrile group ionic liquid-palladium catalyst for synthesizing polyketone and preparation method thereof

A technology of ionic liquid and activated carbon, which is applied in the field of catalysts for the synthesis of polyketones, can solve problems such as wear, loss of metal ions, and reduced catalytic activity, and achieve the effects of large contact area, increased reactivity, and avoiding agglomeration

Active Publication Date: 2012-08-08
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when activated carbon is used as a carrier, the immobilization method belongs to physical adsorption, and the catalytically active species Pd 2+ The crystallites are generally only distributed in the micropores close to the carbon surface, causing any direct friction of the particles to cause wear and also cause metal ion Pd 2+ loss, and the generated product polyketone will cover the pores of activated carbon and embed the active species Pd 2+ , reducing the catalytic activity

Method used

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  • Activated carbon-supported nitrile group ionic liquid-palladium catalyst for synthesizing polyketone and preparation method thereof
  • Activated carbon-supported nitrile group ionic liquid-palladium catalyst for synthesizing polyketone and preparation method thereof
  • Activated carbon-supported nitrile group ionic liquid-palladium catalyst for synthesizing polyketone and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0014] Weigh 10g of 50-60 mesh activated carbon, add 50mL of hydrochloric acid solution with a mass concentration of 20%, soak for 2h at a temperature of 50°C, add the obtained activated carbon into an ammonia solution with a mass concentration of 2% and heat it to 100°C for 10min, then Add 100mL of deionized water to the activated carbon after suction filtration and heat to 100°C for 10 minutes, then filter with suction and repeat three times to remove Cl - , NH 4 + , then add 100ml of deionized water, 15ml of hydrogen peroxide with a mass concentration of 30% and 5mL of a sodium hypochlorite solution with a mass concentration of 10%, and after treating at room temperature for 4 hours, filter, wash, and vacuum dry at a temperature of 40°C for 12 hours to obtain pretreated activated carbon , sealed and kept for later use.

[0015] Dissolve 0.2g of N-valeronitrile-N'-methylimidazolium hexafluorophosphate ionic liquid and 0.211g of palladium acetate in 15ml of acetone, stir at...

Embodiment 2

[0017] The steps of this example are the same as those in Example 1, except that the amount of N-valeronitrile-N'-methylimidazolium hexafluorophosphate ionic liquid is 0.15 g, and the amount of palladium acetate is 0.1477 g to obtain activated carbon-supported nitrile Ionic liquid catalyst, the theoretical loading mass of the catalyst is 7%Pd-15%[C 4 CNmim] + PF 6 - -1gC(b). The actual loading of palladium was determined to be 5.23% by using a 180-80 polarized Zeeman atomic absorption spectrometer from Hitachi, Japan.

Embodiment 3

[0019] The steps of this example are the same as in Example 1, except that the amount of N-valeronitrile-N'-methylimidazolium hexafluorophosphate ionic liquid is 0.1 g, and the amount of palladium acetate is 0.1055 g to obtain activated carbon-supported nitrile Ionic liquid catalyst, the theoretical loading mass of the catalyst is 5%Pd-10%[C 4 CNmim] + PF 6 - -1gC(c). The actual loading of palladium was determined to be 3.46% by using a 180-80 polarized Zeeman atomic absorption spectrometer from Hitachi, Japan.

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Abstract

The invention discloses an activated carbon-supported nitrile group ionic liquid-palladium (Pd) catalyst for synthesizing polyketone and a preparation method thereof, wherein the homogeneous membrane of palladium acetate and N-valeronitrile-N'-methylimidazolium hexafluorophosphate ionic liquid are supported on pretreated activated carbon. The preparation method comprises the following steps: dissolving palladium acetate and N-valeronitrile-N'-methylimidazolium hexafluorophosphate ionic liquid in solvent acetone to stir, then adding pretreated activated carbon in the solution, continuously stirring, distilling, and drying to obtain the activated carbon-supported nitrile group ionic liquid-Pd catalyst. The invention has the advantages that polar group nitrile groups can increase the bindingforce between ionic liquid and activated carbon, the nitrile group ionic liquid membrane coating activated carbon can increase the dispersivity of Pd<2+>, reduce the loss of Pd<2+>, prevent the product polyketone from blocking the pores of activated carbon, prevent Pd<2+> from being embedded and increase the reactivity of the copolymerization of carbon monoxide and styrene for preparing polyketone.

Description

technical field [0001] The invention relates to an activated carbon-supported nitrile-based ionic liquid phase-palladium catalyst for synthesizing polyketones and a preparation method, which belongs to the catalyst technology for synthesizing polyketones. Background technique [0002] In recent years, supported catalysts have been continuously applied in the preparation of polyketones by the copolymerization of carbon monoxide and styrene. Existing studies have shown that the loading methods used to synthesize polyketones mainly include chemical bonds on the surface of the resin to load the active species Pd. 2+ and activated carbon to physically adsorb Pd 2+ . The previous research work in the laboratory shows that under the same conditions, the method of using activated carbon physical adsorption has higher catalytic activity, easier operation and lower cost. This is due to the fact that activated carbon has developed internal pores and a huge specific surface area, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G67/02
CPCY02P20/54
Inventor 郭锦棠胡光冯亚凯
Owner TIANJIN UNIV
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