Ex-situ pre-reduction and passivation treatment method for acetylene pre-hydrogenation catalyst

A hydrogenation catalyst and passivation treatment technology, applied in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc. Affecting problems such as normal driving, achieving high catalytic activity and selectivity, easy storage and transportation, and good economic benefits

Inactive Publication Date: 2018-08-28
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In industry, two methods are generally used to reduce the catalyst. One is to drive the catalyst directly in the oxidized state. While the hydrogenation reaction is going on, the hydrogen in the cracked gas is used for reduction. The advantage of this method is that it saves the additional catalyst preparation. The reduction process simplifies the process, but the disadvantage is that the initial activity is low, and the alkyne and CO in the cracked gas will affect the reduction of palladium oxide, and the reduction while reacting is easy to cause runaway temperature; the other is to first pass pure hydrogen to the catalyst. Internal in-situ reduction, and then feed the raw material gas for hydrogenation reaction. The advantage is that the catalyst is fully reduced and has high activity. The disadvantage is that reduction equipment needs to be added, and the reduction time is long, which affects the normal start-up.
Based on the advantages and disadvantages of the above two catalyst reduction methods, external pre-reduction is a good choice, but the activity of elemental palladium is very high, and it is easily oxidized in the air, which greatly affects its activity. In order to facilitate storage and transportation, the device Externally reduced catalysts need to be passivated

Method used

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  • Ex-situ pre-reduction and passivation treatment method for acetylene pre-hydrogenation catalyst
  • Ex-situ pre-reduction and passivation treatment method for acetylene pre-hydrogenation catalyst
  • Ex-situ pre-reduction and passivation treatment method for acetylene pre-hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 1g 20-40 mesh Pd-Ag / Al 2 o 3 The catalyst (cat0) was loaded into the reactor for pre-reduction and passivation treatment. At normal pressure, the volumetric space velocity is 3000h -1 of pure H 2 Under the conditions, the temperature was programmed at a rate of 1 °C / min to 130 °C for 3 h, and the H 2 Switch to N 2 , turn off the power supply of the heating mantle and cool down to 50°C to start passivation treatment, and turn on N 2 and 5%O 2 , 95% N 2 passivation of the gas mixture, by adjusting the N2 and the flow rate of mixed gas to adjust the concentration of passivation gas, O 2 The molar concentration was gradually increased from 0.61% to 5.0% through eight gradients, and each concentration was maintained for 30 minutes. After that, the volumetric space velocity is 3000h -1 The air continued to passivate for 10h, and the catalyst cat1 was obtained;

[0035] The molar concentration gradient of oxygen is: 0.61%, 0.97%, 1.27%, 1.75%, 2.13%, 2.42%, 3.2...

Embodiment 2

[0037] The specific implementation process is roughly the same as in Example 1, except that the passivation temperature is constant at 50° C., and the obtained passivated catalyst is cat2.

Embodiment 3

[0039] The specific implementation process is roughly the same as in Example 1, except that the passivation temperature is constant at 30° C., and the obtained passivated catalyst is cat3.

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Abstract

The invention discloses an ex-situ pre-reduction and passivation treatment method for an acetylene pre-hydrogenation catalyst. The ex-situ pre-reduction and passivation treatment method comprises: (1)carrying out pre-reduction treatment on an oxidation-state hydrogenation catalyst using Pd and Ag as active components; and (2) carrying out passivation treatment on the pre-reduced hydrogenation catalyst, wherein the passivation process comprises: cooling to a passivation temperature of 30-50 DEG C under a normal pressure under nitrogen protection, introducing oxygen-containing gas with an oxygen molar concentration of 0.61-5.0%, carrying out passivation for 2.5-5.5 h, introducing air, and continuously carrying out passivation for 9-11 h. According to the present invention, the method has characteristics of simple operation, mild condition and good passivation effect, and the obtained product can stably exist in air, is conveniently stored and transported, is easily reduced by H2 in theraw material gas during the use, and can rapidly provide high activity and high selectivity so as to substantially shorten the start-up time and bring good economic benefits to enterprises.

Description

technical field [0001] The invention relates to an external pre-reduction and passivation treatment method of an acetylene pre-hydrogenation catalyst, in particular to an external pre-reduction and passivation treatment method of an acetylene pre-hydrogenation catalyst with Pd-Ag as an active component. Background technique [0002] The pyrolysis gas produced in the steam cracking process of petroleum hydrocarbons often contains a small amount of impurities such as acetylene, propyne (MA) and propadiene (PD), and their existence will affect the homogeneous polymerization and copolymerization processes used in subsequent sections to varying degrees. high-efficiency polyethylene and polypropylene catalysts. According to the requirements of post-processing procedures such as polyethylene, ethylene-propylene rubber, and polypropylene, the molar concentration of acetylene in polymer grade ethylene must be lower than 5ppm, and the molar concentration of acetylene in ethylene must ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/00B01J37/18B01J23/50C07C7/167C07C11/04
CPCB01J23/50B01J37/00B01J37/18C07C7/167C07C11/04Y02P20/52
Inventor 张谦温钱颖车春霞杨振兴孙锦昌韩伟梁玉龙苟尕莲张峰景喜林常晓昕
Owner PETROCHINA CO LTD
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