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Pd redispersed Pd/MCx supported catalyst and preparation method and application thereof

A supported catalyst and catalyst technology, applied in the direction of physical/chemical process catalysts, dehalogenation preparation, chemical instruments and methods, etc., can solve the problems of unenvironmental protection, unsatisfactory recovery of catalyst activity, low efficiency, etc., and achieve low production costs , excellent selectivity, simple preparation method

Active Publication Date: 2019-06-28
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the above method can redisperse noble metal catalysts, there are many disadvantages, such as low redispersion efficiency, unfriendly atmosphere, ex-situ redispersion, unsatisfactory recovery of catalyst activity after redispersion, etc.

Method used

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  • Pd redispersed Pd/MCx supported catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1 g of fresh Pd / FeC with a Pd loading of 3% x The catalyst was loaded into a fixed-bed reactor, fed with hydrogen and reduced at 250°C for 2 hours. Then feed CFC-115 gas at a reaction temperature of 300°C and a space velocity of 720h -1 The reaction is carried out under the conditions, and the feed molar ratio of CFC-115 raw material to hydrogen is 1:1.5. After 80 hours of reaction, when the conversion rate of CFC-115 is lower than 65%, it is recorded as the sintering deactivation of the catalyst.

[0026] The catalyst deactivated by sintering in O with an oxygen volume content of 8% 2 / N 2 Pd / FeO was obtained by calcination at 450℃ for 0.5h x catalyst, and then 10% CH at 300°C 4 / H 2 Gas mixture (i.e. CH 4 / H 2 In the gas mixture, CH 4 The volume content is 10%) calcined and carbonized for 1h to recover Pd / FeC x The activity of the catalyst, that is, the regenerated catalyst is obtained. Under the same reaction conditions, the hydrodechlorination reaction of...

Embodiment 2

[0029] 1 g of fresh Pd / FeC with a Pd loading of 9% x The catalyst was loaded into a fixed-bed reactor, fed with hydrogen and reduced at 250°C for 2 hours. Then feed CFC-115 gas at a reaction temperature of 300°C and a space velocity of 720h -1 The reaction is carried out under the conditions, and the feed molar ratio of CFC-115 raw material to hydrogen is 1:1.5. After 80 hours of reaction, when the conversion rate of CFC-115 is lower than 65%, it is recorded as the sintering deactivation of the catalyst.

[0030] The catalyst deactivated by sintering in O with an oxygen volume content of 16% 2 / N 2atmosphere and calcination at 400°C for 8h to obtain Pd / FeO x catalyst, and then 20% CH at 650°C 4 / H 2 Restoration of Pd / FeC by Mixed Gas Calcination and Carbonization for 10h x The activity of the catalyst, that is, the regenerated catalyst is obtained. Under the same conditions, the hydrodechlorination reaction of CFC-115 under the action of the regenerated catalyst was ca...

Embodiment 3

[0033] 1 g of fresh Pd / FeC with a Pd loading of 5% x The catalyst was loaded into a fixed-bed reactor, fed with hydrogen and reduced at 250°C for 2 hours. Then feed CFC-115 gas at a reaction temperature of 300°C and a space velocity of 720h -1 The reaction is carried out under the conditions, and the feed molar ratio of CFC-115 raw material to hydrogen is 1:1.5. After 80 hours of reaction, when the conversion rate of CFC-115 is lower than 65%, it is recorded as the sintering deactivation of the catalyst.

[0034] The catalyst deactivated by sintering in O with an oxygen volume content of 6% 2 / N 2 atmosphere and calcination at 500°C for 1 h to obtain Pd / FeO x Catalyst, and then calcination and carbonization at 300 °C for 3 h to recover Pd / FeC x The activity of the catalyst, that is, the regenerated catalyst is obtained. Under the same conditions, the hydrodechlorination reaction of CFC-115 under the action of the regenerated catalyst was carried out again.

[0035] When...

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Abstract

The invention discloses a Pd redispersed Pd / MCx supported catalyst and a preparation method and application thereof. The preparation method of the Pd / MCx supported catalyst comprises the following steps of: placing a Pd / MOx catalyst in a tubular furnace, calcining and carbonizing under the condition of introducing carbon-containing gas, and carbonizing metal oxide MOx in the Pd / MOx catalyst into metal carbide MCx to obtain the Pd / MCx supported catalyst, specifically, the metal M in the Pd / MOx catalyst is one or more of transition metals Mo, Fe, W, Ti, Co, Mn, Nb, V, Ta, Zr and Cr. The Pd / MCx catalyst prepared by the preparation method has high initial catalytic activity, and the sintered catalyst can be regenerated in situ through oxidization-carbonization in a fixed bed reactor, therefore, the Pd particles in the Pd / MCx catalyst can be redispersed through reversible circulation, and the activity of the prepared catalyst is restored; and moreover, the prepared catalyst has higher catalytic activity due to higher Pd dispersion degree.

Description

technical field [0001] The present invention relates to a kind of Pd / MC redispersed by Pd x Supported catalyst and its preparation method and application. Background technique [0002] Supported palladium-based catalyst is a commonly used hydrogenation catalyst, which is widely used in the fields of alkane hydrogenation, olefin hydrogenation, nitro and nitroso hydrogenation, and catalytic selective oxidation. For noble metal catalysts, the dispersion of noble metals is a very important indicator, which directly determines the performance of the catalyst. However, due to long-term use or high temperature during use, sintering deactivation is often caused, resulting in a decrease in catalyst activity. For sintered noble metal catalysts, there is often a lack of in-situ regeneration methods. The most common method is to separate the noble metals in the noble metal catalysts and then re-prepare the catalysts. Obviously, this process is not environmentally friendly, and it wil...

Claims

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Application Information

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IPC IPC(8): B01J27/22B01J27/28B01J38/02B01J38/04B01J38/12C01B32/50C07C5/08C07C17/23C07C19/08
CPCY02P20/584
Inventor 唐浩东党明明张歌珊韩文锋李瑛刘宗健
Owner ZHEJIANG UNIV OF TECH
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