High-dispersion palladium-doped sulfur active carbon catalyst, and preparation method and application thereof

A technology of sulfur activated carbon and highly dispersed palladium, which is applied in the field of highly dispersed palladium-sulfur-doped activated carbon catalysts and its preparation, can solve the problems of easy excessive hydrogenation and low ethylene selectivity, and achieve difficult agglomeration and loss, high catalyst activity, The effect of increasing the utilization rate of atoms

Inactive Publication Date: 2019-12-13
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a highly active noble metal, Pd has been widely used in the selective hydrogenation reaction of acet

Method used

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  • High-dispersion palladium-doped sulfur active carbon catalyst, and preparation method and application thereof
  • High-dispersion palladium-doped sulfur active carbon catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh Na 2 S·9H 2 Dissolve 3.8218g of O in 50mL of deionized water, mix well with 5g of activated carbon, and stir magnetically at a stirring rate of 1000r / min in a water bath at 40°C for 60min. Then transfer to a high-pressure hydrothermal reactor for hydrothermal treatment at 180°C for 40 hours; filter after cooling to room temperature, obtain a filter cake by suction filtration, dry in vacuum at 80°C for 8 hours, and transfer to a quartz boat. Place the quartz boat in a tube furnace under N 2 Under the atmosphere, the temperature was raised to 800°C at a rate of 3°C / min and maintained for 2h. After being cooled to room temperature, it was taken out to obtain sulfur-doped activated carbon. Then spread 1 g of the above-mentioned sulfur-doped activated carbon on a watch glass, and add the chloropalladium acid solution dropwise according to the loading amount of 0.1 wt % until the carrier is just wetted, and stir slightly. After the catalyst uniformly wetted by the c...

Embodiment 2

[0030] Weigh Na 2 S·9H 2 O 3.0580g was dissolved in 50mL of deionized water, mixed evenly with 5g of activated carbon, and magnetically stirred at a stirring rate of 600r / min in a 60°C water bath for 40min. Then transfer to a high-pressure hydrothermal reaction kettle for hydrothermal treatment at 250°C for 30h; filter after cooling to room temperature, and obtain a filter cake by suction filtration, vacuum-dry at 60°C for 10h and transfer to a quartz boat. The quartz boat was placed in a tubular heating furnace, and the temperature was raised to 700 °C at a rate of 3 °C / min under He atmosphere, and maintained for 3 h. After being cooled to room temperature, it was taken out to obtain sulfur-doped activated carbon. Then spread 1 g of the above-mentioned sulfur-doped activated carbon on a watch glass, add palladium acetate solution dropwise according to the load of 0.08 wt% until the carrier is just wet, and stir slightly. After the catalyst uniformly wetted by the chloropal...

Embodiment 3

[0032] Weigh Na 2 S·9H 2 Dissolve 1.9123g of O in 50mL of deionized water, mix well with 5g of activated carbon, and stir magnetically at a stirring rate of 300r / min in a water bath at 80°C for 50min. Then transfer to a high-pressure hydrothermal reactor for hydrothermal treatment at 200°C for 24 hours; filter after cooling to room temperature, and obtain a filter cake by suction filtration, vacuum-dry at 50°C for 12 hours, and then transfer to a quartz boat. The quartz boat was placed in a tubular heating furnace, and the temperature was raised to 600 °C at a rate of 3 °C / min under Ar atmosphere, and maintained for 4 h. After being cooled to room temperature, it was taken out to obtain sulfur-doped activated carbon. Then spread 1 g of the above-mentioned sulfur-doped activated carbon on a watch glass, and add the chloropalladium acid solution dropwise according to the loading amount of 0.05 wt % until the carrier is just wetted, and stir slightly. After the catalyst unifor...

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Abstract

The invention provides a high-dispersion palladium-doped sulfur active carbon catalyst, and a preparation method and application thereof. According to the preparation method, sulfur doping is carriedout by adopting a method of carrying out a hydrothermal process first and then carrying out roasting, and the doped sulfur can more stably exist on the surface of a carbon material by the method. A method for loading noble metal by an impregnation method is simple and convenient, and cost is low. In the high-dispersion palladium-doped sulfur active carbon catalyst, doped sulfur on the surface of the carrier exerts an anchoring effect, so that high dispersion and size regulation and control of palladium nanoparticles can be realized, and the atom utilization rate of a noble metal is effectivelyimproved. Strong interaction between sulfur and the metal ensures high stability of the catalyst, so that the metal nanoparticles are not easily agglomerated or lost in an acetylene hydrogenation reaction process, and the service life of the catalyst is prolonged. The catalyst disclosed by the invention has high selectivity to ethylene in an acetylene hydrogenation reaction, and acetylene can becompletely converted. In addition, the use condition is mild, stability is good, the usage amount of the catalyst is small, and the service life of the catalyst is long.

Description

[0001] (1) Technical field [0002] The invention relates to a high-dispersion palladium-sulfur-doped activated carbon catalyst and a preparation method thereof, as well as an application in the reaction of acetylene selective hydrogenation to prepare ethylene. [0003] (2) Background technology [0004] Ethylene is an important raw material for industrial organic synthesis, mainly used for large-scale production of polyethylene, polyvinyl chloride, ethylene oxide, ethanol, acetaldehyde, etc. Because of the wide range of uses of ethylene, there is a huge demand for its production in industry. Ethylene is mainly derived from the cracking of naphtha, and acetylene is inevitably produced as a by-product during this process, and the oligomers formed by the polymerization of acetylene will seriously poison the downstream ethylene polymerization catalyst. Industrial ethylene feed gas often contains 1% acetylene. Therefore, the selective removal of a small amount of residual acetyle...

Claims

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Application Information

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IPC IPC(8): B01J27/02B01J23/44C07C7/167C07C11/04
CPCB01J27/02B01J23/44C07C7/167C07C2527/02C07C2523/44C07C11/04Y02P20/52
Inventor 张群峰周媛张超杰马磊卢春山丰枫吕井辉李小年
Owner ZHEJIANG UNIV OF TECH
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