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Sulfur-doped carbon material loading noble-metal catalyst and application thereof

A technology of noble metal catalysts and carbon materials, which is applied in the direction of physical/chemical process catalysts, organic chemistry, amino compound preparation, etc., can solve the problems of reducing the purity and quality of hydrogenation products, complex operations, etc., to avoid sulfur loss, high activity, highly selective effect

Active Publication Date: 2016-12-07
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this regeneration method has complex operations, and the desorbed sulfides reduce the purity and quality of hydrogenation products.

Method used

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  • Sulfur-doped carbon material loading noble-metal catalyst and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Weigh 10g of activated carbon, the particle size of activated carbon is 150 mesh, and the specific surface area is 1400m 2 / g, the ash content is 0.5wt%, it is mixed evenly with 0.7g elemental sulfur, and treated at 1000°C for 5h under nitrogen atmosphere to obtain sulfur-doped activated carbon. Then the above-mentioned sulfur-doped activated carbon was prepared into a slurry at a temperature of 70° C. in 100 ml of deionized water, and 10 ml of H 2PdCl 4 solution (the Pd content is 0.04g / ml), stirred for 2.5h; the pH value of the solution was adjusted to 8 with 10wt% NaOH solution, and the temperature was lowered to room temperature, filtered, and the filter cake was washed to neutrality with deionized water; The filter cake was configured into a slurry at 70°C, 2ml of 85% hydrazine hydrate solution was added dropwise, stirred for 2 hours, filtered, the filter cake was washed with deionized water until neutral, and vacuum-dried at 100°C to obtain sulfur-doped activated...

Embodiment 2

[0042] Weigh 10g of activated carbon, the particle size of activated carbon is 300 mesh, and the specific surface area is 1200m 2 / g, ash content 0.3wt%, put it in H 2 S / Ar mixed gas (volume ratio 1 / 10) was treated at 800° C. for 10 h at a mixed gas flow rate of 2 L / h to obtain sulfur-doped activated carbon. The above-mentioned sulfur-doped activated carbon was prepared into a slurry at a temperature of 60°C in 100ml of deionized water, and 8ml of H 2 PtCl 6 solution (Pt content is 0.05g / ml), stirred for 2h; the pH value of the solution was adjusted to 8.5 with 10wt% KOH solution, and the temperature was lowered to room temperature, filtered, and the filter cake was washed to neutrality with deionized water; The cake was prepared into a slurry at 60°C, 10ml of formaldehyde was added dropwise, stirred for 2 hours, filtered, the filter cake was washed with deionized water until neutral, and dried in vacuum at 90°C to obtain a platinum catalyst supported on sulfur-doped activat...

Embodiment 3

[0044] Weigh 10g of activated carbon, the particle size of activated carbon is 400 mesh, and the specific surface area is 1600m 2 / g, the ash content is 1.0wt%, it is mixed with 4g of thiophene evenly, and treated at 600°C for 3h under helium atmosphere to obtain sulfur-doped activated carbon. The above sulfur-doped activated carbon was prepared into a slurry at a temperature of 40°C in 100ml of deionized water, and 10ml of Pd(NO 3 ) 2 solution (with a Pd content of 0.05g / ml), stirred for 4h; the pH value of the solution was adjusted to 9 with ammonia water, and the temperature was lowered to room temperature, filtered, and the filter cake was washed with deionized water until neutral; Prepare a slurry under water, add 30ml of formic acid dropwise, stir for 4 hours, filter, wash the filter cake with deionized water until neutral, and dry it in vacuum at 80°C to obtain a sulfur-doped activated carbon-supported palladium catalyst.

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Abstract

The invention relates to a sulfur-doped carbon material loading noble-metal catalyst and an application thereof. The catalyst contains noble metal, i.e., Pt or Pd and is prepared by a preparation method comprising the following steps: (1) obtaining a sulfur-doped carbon material; (2) preparing slurry with the temperature of 20 DEG C to 95 DEG C from the sulfur-doped carbon material, dropwise adding a solution of a soluble noble-metal compound into the slurry slowly, and carrying out uniform stirring thoroughly; carrying out dipping while carrying out heat preservation, then, adding an alkaline solution to adjust the pH value to 7.0 to 10.0, cooling the mixture to room temperature, carrying out filtering, and washing the filter cake with deionized water until the filter cake is neutral; preparing slurry from the filter cake at the temperature of 20 DEG C to 95 DEG C, dropwise adding a liquid-phase reducer into the slurry, carrying out a reduction reaction with stirring, carrying out filtering after the reaction ends, and subjecting the filter cake to water washing and drying, thereby obtaining the sulfur-doped carbon material loading noble-metal catalyst. The catalyst provided by the invention shows the characteristics of high activity, high selectivity and high stability in the application of a reaction for synthesizing a rubber anti-aging agent 4020 from an RT base and MIBK, which serve as raw materials, by a one-step method or two-step method.

Description

(1) Technical field [0001] The invention relates to a sulfur-doped carbon material supported noble metal catalyst and its application in catalytic reduction alkylation synthetic rubber antioxidant 4020. (2) Background technology [0002] P-phenylenediamine rubber antioxidants are widely used because of their good protective properties. They are generally prepared from p-aminodiphenylamine (RT base) and aliphatic ketones through reductive alkylation. Among them: anti-aging agent 4020, the scientific name is N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine, which is the most commonly used rubber anti-aging agent at present. It is made of raw material N-phenyl-p-phenylenediamine Amine (RT base) and methyl isobutyl ketone (MIBK), under the action of a catalyst, prepared by hydrodehydration reaction, the reaction equation is as follows: [0003] [0004] The catalysts used in the synthesis of p-phenylenediamine rubber antioxidants mainly include carbon-supported noble metal...

Claims

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Application Information

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IPC IPC(8): B01J27/045C07C209/78C07C211/55
CPCB01J27/045C07C209/78C07C211/55
Inventor 李小年张群峰丰枫马磊卢春山许孝良
Owner ZHEJIANG UNIV OF TECH
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