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Method for sulfurizing shift catalyst in process of preparing methanol from coal

A conversion catalyst, coal-to-methanol technology, applied in physical/chemical process catalysts, catalyst activation/preparation, chemical instruments and methods, etc., to achieve the effects of easy operation, reduced safety hazards, and reduced vulcanization costs

Active Publication Date: 2016-10-12
HENAN LONGYU COAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is: aiming at the inadequacies existing in the catalyst sulfuration reaction process of the current shift furnace before the first gas connection, the present invention provides a sulfuration method of the shift catalyst in the coal-to-methanol process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The vulcanization method of conversion catalyst in the coal-to-methanol process of the present invention, the detailed steps of described vulcanization method are as follows:

[0040] (1) The temperature rise of the catalyst:

[0041] a. First, replace the converter furnace and the nitrogen heating system. When the gas analysis index at the outlet of the converter furnace reaches O 2 The replacement ends when the volume content is ≤0.1%;

[0042] b. Use pure nitrogen to raise the temperature of the catalyst bed at a heating rate of 40°C / h (in the process of heating up, discharge the condensed water from the nitrogen separator, and collect and measure the water; in each constant temperature stage, the water must be completely drained, and the bed The next step can only be carried out after the temperature of each point is equalized); when the inlet temperature of the catalyst bed rises to 230°C and the lowest temperature of the bed reaches 210°C, the temperature rise of...

Embodiment 2

[0057] The vulcanization method of conversion catalyst in the coal-to-methanol process of the present invention, the detailed steps of described vulcanization method are as follows:

[0058] (1) The temperature rise of the catalyst:

[0059] a. First, replace the converter furnace and the nitrogen heating system. When the gas analysis index at the outlet of the converter furnace reaches O 2 The replacement ends when the volume content is ≤0.1%;

[0060] b. Use pure nitrogen to raise the temperature of the catalyst bed at a heating rate of 35°C / h (in the process of heating up, discharge the condensed water from the nitrogen separator, and collect and measure the water; in each constant temperature stage, the water must be completely drained, and the bed The next step can only be carried out after the temperature of each point is equalized); when the inlet temperature of the catalyst bed rises to 230°C and the lowest temperature of the bed reaches 210°C, the temperature rise of...

Embodiment 3

[0075] The vulcanization method of conversion catalyst in the coal-to-methanol process of the present invention, the detailed steps of described vulcanization method are as follows:

[0076] (1) The temperature rise of the catalyst:

[0077] a. First, replace the converter furnace and the nitrogen heating system. When the gas analysis index at the outlet of the converter furnace reaches O 2 The replacement ends when the volume content is ≤0.1%;

[0078] b. Use pure nitrogen to raise the temperature of the catalyst bed at a heating rate of 45°C / h (in the process of heating up, discharge the condensed water from the nitrogen separator, and collect and measure the water; in each constant temperature stage, the water must be completely drained, and the bed The next step can only be carried out after the temperature of each point is equalized); when the inlet temperature of the catalyst bed rises to 230°C and the lowest temperature of the bed reaches 210°C, the temperature rise of...

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Abstract

The invention discloses a method for sulfurizing a shift catalyst in a process of preparing methanol from coal. The method comprises the following steps: displacing a shift converter and a nitrogen heating system, and heating a catalyst bed by adopting pure nitrogen; performing initial sulfurization after heating: starting hydrogen addition to increase the hydrogen concentration to 25 percent by virtue of purge gas, starting supplementing CS2, and performing initial sulfurization for 14 to 18h; then performing main sulfurization: increasing the addition amounts of the purge gas and the CS2, and raising the temperature of the catalyst bed for main sulfurization; performing final sulfurization after main sulfurization is continuously performed for 12 to 14h: increasing the addition amounts of the purge gas and the CS2, and when results obtained by continuously analyzing the volume concentration of H2S at an outlet for three times all reach 50 to 65g / m<3>, ending sulfurization of the catalyst; performing cooling treatment, and ending the whole sulfurization process. According to the method, the phenomenon of overheat caused by drastic heat release reaction of pure hydrogen in the heating sulfurization process of the catalyst can be avoided, so that reaction of the bed can be steadily performed.

Description

1. Technical field: [0001] The invention belongs to the technical field of sulfur-resistant shift catalysts, and in particular relates to a sulfuration method for shift catalysts in the coal-to-methanol process. 2. Background technology: [0002] In the production process of the coal-to-methanol united acetic acid unit, the converter needs to carry out catalyst vulcanization work before the first gas connection, but the current domestic catalyst heating and vulcanization methods are all using CS 2 and H 2 . The main chemical reactions in the vulcanization process are as follows: [0003] CoO+H 2 S→CoS+H 2 O ΔH 0 298 =-13.4KJ / mol (1) [0004] MoO 3 +2H 2 S+H 2 →MoS 2 +3H 2 O ΔH 0 298 =-48.1KJ / mol (2) [0005] CS 2 +4H 2 →2H 2 S+CH 4 ΔH 0 298 =-240.6KJ / mol (3) [0006] The above reactions are all exothermic reactions, and the hydrogenolysis reaction (3) is a strongly exothermic reaction. In the process of using pure hydrogen to heat up and sulfide the c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/20
CPCB01J37/20
Inventor 崔发科牛玉奇谢肥东刘继铮杜霞沈小炎李星黄孺国李磊
Owner HENAN LONGYU COAL CHEM
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