A kind of in-situ regeneration method of PD catalyst for CO dehydrogenation purification

An in-situ regeneration and catalyst technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problems of increasing regeneration costs and achieve in-situ regeneration , good regeneration effect

Active Publication Date: 2019-05-17
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The regeneration method of the above patent needs to introduce chlorine-containing organic matter or acid treatment catalyst to remove H from CO gas 2 The reaction is a gas-solid reaction, and the device is a fixed-bed reaction device. If the above-mentioned organic matter or acid is used to regenerate the deactivated catalyst, the catalyst needs to be removed from the reaction tube, or the reaction device must be modified to add a liquid sampling pump and a vaporization chamber. and other additional devices, thereby increasing the cost of regeneration

Method used

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  • A kind of in-situ regeneration method of PD catalyst for CO dehydrogenation purification
  • A kind of in-situ regeneration method of PD catalyst for CO dehydrogenation purification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In the CO gas dehydrogenation reactor, N 2 Pass it into the reaction tube containing the deactivated catalyst and purge for 12h at 100℃, N 2 The airspeed is 1000h -1 ; Raise the reaction temperature to 700°C and pass O 2 With N 2 The mixed gas is oxidized for 12h, and the space velocity of the mixed gas is 1000h -1 , O 2 The content is 50%; after the oxidation treatment, at this temperature, pass in HCl and N 2 The mixed gas is chlorinated for 5h, and the space velocity of the mixed gas is 1000h -1 , The content of HCl gas is 5%; after the chlorination treatment, the reaction device is cooled to 400°C, and H 2 With N 2 The mixed gas is reduced for 5h, and the space velocity of the mixed gas is 1000h -1 , H 2 The content is 50%; after the reduction is completed, pass into N 2 Lower the reaction device to room temperature, N 2 Airspeed is 1000h -1 , Complete regeneration.

[0025] The performance evaluation of the regenerated catalyst, the residual H after the reaction 2 The co...

Embodiment 2

[0027] The regeneration process is the same as in Example 1, except that the inert gas He replaces N in the process. 2 Processing 3h, the airspeed of He is 500h -1 ; The oxidation conditions are: T=200℃, the space velocity is 100h -1 Pure O 2 Oxidation treatment is 1h instead of T=700℃, the space velocity is 1000h -1 O 2 The mixed gas with a content of 50% is treated for 12 hours.

[0028] The performance evaluation of the regenerated catalyst, the residual H after the reaction 2 The content is 32 ppm and the selectivity is 69.8%. Through static CO chemisorption detection, the Pd dispersion of the regenerated catalyst was 40.5%, and the average Pd particle size was 2.5 nm.

Embodiment 3

[0030] Same as the regeneration process of Example 1, the difference is that the inert gas Ar replaces N in the process 2 ; The chlorination condition is: the space velocity is 100h -1 HCl content of 10% mixed gas chlorination treatment 1h instead of 1000h space velocity -1 The mixed gas with HCl content of 5% is chlorinated for 5h.

[0031] The performance evaluation of the regenerated catalyst, the residual H after the reaction 2 The content is 76 ppm and the selectivity is 63.7%. Through static CO chemical adsorption detection, the Pd dispersion of the regenerated catalyst was 25.7%, and the average Pd particle size was 4.1 nm.

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Abstract

The invention discloses an in-situ regeneration method of a Pd catalyst for CO dehydrogenation purification after inactivation, wherein the method comprises the following particular steps: introducing N2, and purging to remove adsorbed substances on the surface of the catalyst; introducing O2, and oxidizing agglomerated Pd on the surface of the catalyst; introducing HCl or Cl2, and redispersing active components; and introducing H2, reducing, and carrying out dechlorination treatment to complete regeneration. The regeneration process takes place in situ in a dehydrogenation reaction device, and devices are not needed to be additionally constructed. According to the catalyst after regeneration treatment, the Pd metal dispersion degree and the catalytic effect are significantly improved, the selectivity can be restored to more than or equal to 80% of the fresh catalyst, and H2 can be removed to 100 ppm or less. The regeneration method is mainly applied in an industrial CO gas dehydrogenation purification process.

Description

Technical field [0001] The invention relates to an in-situ regeneration method of a deactivated Pd catalyst, which is applied to an industrial CO gas dehydrogenation purification process. Background technique [0002] During the operation of industrial catalysts, it is inevitable that as the reaction time increases, the activity and selectivity of the catalyst will gradually decrease, and the efficiency of the catalyst will continue to decrease and eventually become deactivated. The main types of catalyst deactivation are divided into coke deactivation, poisoning deactivation and sintering deactivation. Generally, in order to ensure the stable operation of the reaction in the industrial production process, the catalyst must be replaced regularly. Because precious metal resources are scarce and relatively expensive, for precious metal catalysts, catalyst regeneration can realize the reuse of precious metals, reduce the frequency of catalyst replacement, and greatly save the opera...

Claims

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Application Information

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IPC IPC(8): B01J37/14B01J37/24B01J37/18B01J23/96B01J23/44C01B32/40
CPCY02P20/584
Inventor 姚元根宗珊珊周张锋乔路阳崔国静吴小满吴娟
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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