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Preparation method and application of a sulfur-modified activated carbon-supported noble metal catalyst

A noble metal catalyst and activated carbon technology, which is applied in the field of preparation of sulfur-modified activated carbon-supported noble metal catalysts, can solve the problems of low activity of noble metal sulfide catalysts, and achieve the effect of improving selectivity, increasing selectivity, and high catalytic activity

Active Publication Date: 2021-10-15
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the activity of noble metal sulfide catalysts is low

Method used

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  • Preparation method and application of a sulfur-modified activated carbon-supported noble metal catalyst
  • Preparation method and application of a sulfur-modified activated carbon-supported noble metal catalyst
  • Preparation method and application of a sulfur-modified activated carbon-supported noble metal catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Weigh 10g of activated carbon with a particle size of 800 mesh and a specific surface area of ​​1000m 2 / g, the pore volume is 0.6ml / g, configure 6ml containing Na 2 S solution (the concentration of S in the solution is 0.0333g / ml, and the S content is 0.2g); the impregnated activated carbon is vacuum-dried at 100°C for 10h.

[0031] (2) Configure 6ml containing H 2 PdCl 4 (the concentration of Pd in ​​the solution is 0.0333g / ml, and the Pd content is 0.2g), and the solution is added dropwise to the activated carbon loaded with sulfur obtained in step (1), and stirred evenly. The impregnated catalyst was vacuum-dried at 60 °C for 8 h.

[0032] (3) the activated carbon of the loaded sulfur and noble metal that step (2) obtains, in H 2 The reduction was carried out at 150° C. for 3 hours under the atmosphere, that is, the sulfur-modified activated carbon supported palladium catalyst.

Embodiment 2

[0034] (1) Weigh 10g of activated carbon with a particle size of 100 mesh and a specific surface area of ​​2000m 2 / g, the pore volume is 0.8ml / g, configure 8ml containing K 2 S solution (the concentration of S in the solution is 0.025g / ml, and the S content is 0.2g); the impregnated activated carbon is vacuum-dried at 150°C for 6h.

[0035] (2) Configure 8ml containing H 2 PtCl 6 (the concentration of Pt in the solution is 0.05g / ml, and the Pt content is 0.4g), and the solution is added dropwise to the activated carbon loaded with sulfur obtained in step (1), and stirred evenly. The impregnated catalyst was vacuum-dried at 80 °C for 4 h.

[0036] (3) the activated carbon of the loaded sulfur and noble metal that step (2) obtains, in H 2 The reduction was carried out at 120°C for 5 hours under the atmosphere, that is, the platinum catalyst supported on sulfur-modified activated carbon.

Embodiment 3

[0038] (1) Weigh 10g of activated carbon with a particle size of 1000 mesh and a specific surface area of ​​600m 2 / g, the pore volume is 0.3ml / g, configure 3ml containing Na 2 S solution (the concentration of S in the solution is 0.01g / ml, and the S content is 0.03g); the impregnated activated carbon is vacuum-dried at 200°C for 4h.

[0039] (2) Configure 3ml containing Pd(NO 3 ) 2solution (the concentration of Pd in ​​the solution is 0.0333g / ml, and the Pd content is 0.1g), and the solution is added dropwise to the activated carbon loaded with sulfur obtained in step (1), and stirred evenly. The impregnated catalyst was vacuum dried at 40°C for 10 h.

[0040] (3) The activated carbon loaded with sulfur and noble metals obtained in step (2) was reduced for 10 h at 80° C. under H2 atmosphere, that is, the sulfur-modified activated carbon supported palladium catalyst.

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Abstract

The invention discloses a preparation method and application of a sulfur-modified activated carbon-supported noble metal catalyst. The preparation method is carried out according to the following steps: (1) take activated carbon and impregnate the sulfur-containing compound Na 2 S or K 2 S, so that the sulfur load is 0.1-4%, vacuum-dry the impregnated activated carbon at 90-200°C for 4-10 hours to obtain sulfur-loaded activated carbon; (2) impregnate the sulfur-loaded activated carbon with an equal volume Impregnating noble metal compounds by impregnation method, the noble metal is Pd or Pt, so that the load of noble metal is 0.5-10wt%, and the impregnated activated carbon is vacuum-dried at 40-80°C for 4-10 hours to obtain activated carbon loaded with sulfur and noble metal ; (3) Activated carbon loaded with sulfur and precious metals, in H 2 Reduction is carried out at 80-160° C. for 3-10 hours under atmosphere to obtain a sulfur-modified activated carbon-supported noble metal catalyst. The invention provides the application of the catalyst in selective hydrogenation reaction, which has high catalytic activity and target product selectivity.

Description

(1) Technical field [0001] The invention relates to a preparation method of a sulfur-modified activated carbon supported noble metal catalyst and its application in selective hydrogenation reaction. (2) Background technology [0002] Supported noble metal catalysts such as Pt and Pd are widely used in various organic synthesis reactions due to their high activity and easy separation and recovery. However, when the selective hydrogenation reduction of substances with multiple reducing functional groups is carried out, too high catalytic activity often causes excessive hydrogenation in the reaction, which cannot meet the requirement of high selectivity. The use of noble metal sulfide catalysts is an effective way to obtain high selectivity. This type of catalyst shows better selectivity and stability in hydrogenation reaction. However, the activity of noble metal sulfide catalysts is relatively low. [0003] Therefore, it is very meaningful to search for a hydrogenation cat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/42B01J23/44B01J37/02B01J37/18B01J37/20C07B43/04C07C209/36C07C211/52C07C213/02C07C217/84C07C227/04C07C229/60C07C303/22C07C309/46
CPCB01J23/42B01J23/44B01J35/006B01J37/0207B01J37/024B01J37/18B01J37/20C07B43/04C07C209/365C07C213/02C07C227/04C07C303/22C07C211/52C07C217/84C07C229/60C07C309/46
Inventor 张群峰周媛丰枫马磊卢春山李小年
Owner ZHEJIANG UNIV OF TECH
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