A kind of palladium/carbon material catalyst preparation method and application of carbon material in situ immobilized palladium nanoparticles

A carbon material, palladium nanotechnology, applied in the field of catalyst preparation, can solve the problems of high cost, inconsistent with the development concept of green chemical industry, large pollution, etc., and achieve the effect of no reduction in activity

Active Publication Date: 2021-06-01
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method can control the palladium nanoparticles below 3nm, but the use of organic solvents in the emulsifier causes the method to have high cost and great pollution, which does not conform to the development concept of green chemical industry

Method used

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  • A kind of palladium/carbon material catalyst preparation method and application of carbon material in situ immobilized palladium nanoparticles
  • A kind of palladium/carbon material catalyst preparation method and application of carbon material in situ immobilized palladium nanoparticles
  • A kind of palladium/carbon material catalyst preparation method and application of carbon material in situ immobilized palladium nanoparticles

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1, 50ml of acetic acid was added to 500ml of deionized water, stirred for 5min to prepare an aqueous solution of acetic acid; step 2, 50mg of palladium acetate and 500mg of carbon black were placed in the aqueous solution of acetic acid prepared in step 1, and evenly stirred for 60min to prepare To obtain a mixed solution, step 3, place the mixed solution prepared in step 2 for ultrasonic dispersion in an ultrasonic cleaning machine, control the time at 100min, and control the ultrasonic power at 400W, take it out and then stir for 60min; step 4, prepare the mixed solution obtained in step 3 The final dispersion was placed in a rotary evaporator at 90°C and dried for 24 hours to prepare a palladium / carbon black catalyst in which carbon black supported palladium nanoparticles in situ. From the XRD pattern of the sample, such as figure 1 As shown, it can be seen that (111), (200), (220), (311), (222) characteristic diffraction peaks of palladium and (002) graphite br...

Embodiment 2

[0023] Step 1, 30ml of acetic acid was added to 350ml of deionized water, stirred for 5min to obtain an aqueous solution of acetic acid; step 2, 40mg of palladium acetate and 300mg of carbon nanotubes were placed in the aqueous solution of acetic acid prepared in step 1, and stirred evenly for 60min, Prepare the mixed solution, step 3, place the mixed solution prepared in step 2 in an ultrasonic cleaner for ultrasonic dispersion, control the time at 100min, control the ultrasonic power at 400W, take it out and then stir for 60min; step 4, prepare the mixed solution in step 3 The mixed dispersion was placed in a rotary evaporator at 60° C. and dried for 36 hours to prepare a palladium / carbon nanotube catalyst in which palladium nanoparticles were immobilized on carbon nanotubes in situ. From the XRD pattern of the sample, such as figure 2 As shown, it can be seen that (111), (200), (220), (311) characteristic diffraction peaks of palladium and (002) characteristic peaks of car...

Embodiment 3

[0025] Step 1, 20ml of acetic acid is added to 200ml of deionized water, stirred for 5min to prepare an aqueous solution of acetic acid; step 2, 20mg of palladium acetate and 150mg of graphene are placed in the aqueous solution of acetic acid prepared in step 1, stirred evenly for 60min to prepare To obtain a mixed solution, step 3, place the mixed solution prepared in step 2 for ultrasonic dispersion in an ultrasonic cleaning machine, control the time at 100min, and control the ultrasonic power at 350W, take it out and then stir for 60min; step 4, prepare the mixed solution obtained in step 3 The final dispersion was placed in a rotary evaporator at 90° C. and dried for 18 hours to prepare a palladium / graphene catalyst in which palladium nanoparticles were immobilized on graphene in situ. From the XRD pattern of the sample, such as Figure 5 As shown, it can be seen that the (111), (200), (220) characteristic diffraction peaks of palladium and the (002) graphite broad peak of...

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Abstract

The invention relates to the technical field of catalyst preparation, a preparation method and application of a palladium / carbon material catalyst in which carbon materials in situ immobilize palladium nanoparticles, wherein the preparation method comprises the following steps: (1) adding acetic acid into water, stirring to prepare To obtain an aqueous solution of acetic acid, (2) place palladium acetate and carbon material in the aqueous solution of acetic acid, and stir uniformly to obtain a mixed solution, (3) place the mixed solution prepared in step 2 to ultrasonically disperse in an ultrasonic cleaning machine, and stir after taking it out , (4) The mixed dispersion obtained in step 3 is placed in a rotary evaporator, and dried to obtain a palladium / carbon material catalyst of carbon material in-situ immobilized palladium nanoparticles. The method of the invention has the characteristics of less energy consumption, low cost, environmental friendliness, and easy large-scale use. The prepared palladium / carbon catalyst is applied to the reaction of preparing benzaldehyde by the selective oxidation of benzyl alcohol, and the conversion rate of benzyl alcohol into benzaldehyde It can reach 96%‑99.3%, and the selectivity can reach 98%‑100%.

Description

technical field [0001] The invention relates to a preparation method and application of a palladium / carbon material catalyst in which carbon materials in situ immobilize palladium nanoparticles, and belongs to the technical field of catalyst preparation. Background technique [0002] Palladium / carbon catalyst plays an important role in petrochemical, fine chemical and organic synthesis due to its high catalytic activity and good selectivity. Since it was discovered in 1872 that palladium / carbon can catalyze the nitro hydrogenation reduction reaction on the benzene ring, palladium / carbon catalytic hydrogenation has the advantages of high conversion rate, high yield, simple process and less waste, etc., which has attracted much attention. great attention of researchers and industry. [0003] At present, the preparation methods of palladium / carbon catalyst mainly include: chemical reduction method, biological reduction method, ultrasonic nanometer metal loading method, plasma ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J35/06B01J37/34C07C47/54C07C45/29
CPCB01J23/44B01J35/0013B01J35/006B01J35/0093B01J35/06B01J37/343C07C45/29C07C47/54
Inventor 邱介山姚秀超于畅倪林魏千兵
Owner DALIAN UNIV OF TECH
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