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Iron catalyst for slurry reactor hydrogenation, preparation, design method, and applications thereof

A catalyst, slurry bed technology, applied in catalyst activation/preparation, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc. Difficult to recycle and other problems, to achieve the effect of easy attachment to the carrier, good catalytic activity, and strong catalytic effect

Inactive Publication Date: 2015-08-12
CATECH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, for heavy crude oil, low-quality heavy oil hydrogenation process, oil-coal mixing process and direct coal liquefaction process, due to the limitation of process and raw materials, there are many solid products, and the catalyst is difficult to recycle. At present, most of them are waste after reaction. directly discarded together, and the existing catalyst precious metal content is high, so the production cost is very high
The unsatisfactory comprehensive performance of the current catalysts limits its application in the above fields

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0039] Example 1: Hydrogenation test of residual oil

[0040] (1) Configure FeSO with a concentration of 40% 4 aqueous solution;

[0041] (2) inject ammoniacal liquor in the solution that step 1 makes, and ammoniacal liquor concentration is 2.0wt%, generates Fe(OH) 2 and (NH4) 2 SO 4 The slurry, PH=7.0;

[0042] (3) feed air into the slurry that step 2 makes, Fe(OH) 2 Oxidation to FeOOH (iron oxyhydroxide), the reaction temperature is 45 ° C, PH = 6.8;

[0043] (4) filter the slurry prepared in step 3 to obtain a filter cake whose main component is FeOOH;

[0044] (5) Add deionized water to the filter cake prepared in step 4 and stir evenly to make a slurry;

[0045] (6) Add 10% ammonium molybdate solution to the slurry prepared in step 5, and stir evenly. The amount of addition is 1:500 based on the amount of Mo / Fe material, stirring and mixing;

[0046] (7) Add dry coal powder ground to 50 μm into the slurry prepared in step 6, and stir evenly. The amount added is ...

example 2

[0055] Example 2: Coal direct liquefaction test

[0056] (1) The configuration concentration is 20wt% FeSO 4 aqueous solution;

[0057] (2) inject ammoniacal liquor in the solution that step 1 makes, and ammoniacal liquor concentration is 1.0wt%, generates Fe(OH) 2 and (NH 4 ) 2 SO 4 The slurry, PH=5.0;

[0058] (3) feed air into the slurry that step 2 makes, Fe(OH) 2 Oxidation into FeOOH (iron oxyhydroxide) precipitation, the reaction temperature is 20 ° C, PH = 6.0;

[0059] (4) The slurry obtained in step 3 is filtered and washed to remove (NH 4 ) 2 SO 4 , to obtain a filter cake whose main component is FeOOH;

[0060] (5) add distilled water and stir in the filter cake that step 4 makes, make slurry;

[0061] (6) Add 20% ammonium molybdate aqueous solution to the slurry prepared in step 5, stir evenly, the scope of the amount added is calculated as 1 / 600 with the amount of Mo / Fe material, stir and mix;

[0062] (7) Add the active carbon powder of particle diame...

example 3

[0071] Example 3: Oil-coal mixing test

[0072] (1) The configuration concentration is 60wt% FeSO 4 aqueous solution;

[0073] (2) inject ammoniacal liquor in the solution that step 1 makes, and ammoniacal liquor concentration is 5.0wt%, generates Fe(OH) 2 and (NH 4 ) 2 SO 4 The slurry, PH=7.5;

[0074] (3) feed air into the slurry that step 2 makes, Fe(OH) 2 Oxidation into FeOOH (iron oxyhydroxide) precipitation, the reaction temperature is 20 ° C, PH = 9.0;

[0075] (4) The slurry obtained in step 3 is filtered and washed to remove (NH 4 ) 2 SO 4 , to obtain a filter cake whose main component is FeOOH;

[0076] (5) add distilled water and stir in the filter cake that step 4 makes, make slurry;

[0077] (6) Add 10wt% ammonium molybdate aqueous solution to the slurry prepared in step 5, stir evenly, the range of the amount added is calculated as 1 / 300 with the amount of Mo / Fe material, stir and mix;

[0078] (7) Add dry coal powder with a particle size of 150 μm to...

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Abstract

The invention discloses an iron catalyst for slurry reactor hydrogenation, preparation, a design method, and applications thereof. The iron catalyst comprises the following components: iron main catalyst (FeOOH), an active auxiliary agent (ammonium molybdate), and a carrier (dry coal powder or active carbon powder); wherein the mass ratio of metal center (Mo) to Fe is 1:350 to 1:175, and the mass ratio of metal center (Fe) to carrier is 1:30 to 1:3. The preparation method comprises the following steps: dissolving FeOOH into distilled water, evenly stirring to obtain FeOOH slurry; adding an ammonium molybdate water solution into the FeOOH slurry, evenly stirring to obtain FeOOH slurry with dispersed molybdenum; adding a carrier into the FeOOH slurry with dispersed molybdenum, evenly stirring, filtering to obtain filter cakes; drying the filter cakes in the atmosphere of N2, and grinding the filter cakes to a size of 10-200 [mu]m to obtain the iron catalyst for slurry reactor hydrogenation. The provided iron catalyst can be applied to residual oil hydrogenation, direct coal liquefaction, and oil-coal blending, the conversion rate and liquid yield are both very high, and the economic benefits are prominently improved.

Description

technical field [0001] The invention relates to a catalyst for slurry bed hydrogenation, in particular to an iron-based catalyst and its preparation, design method and application, and belongs to the fields of petrochemical and coal chemical industries. Background technique [0002] In recent years, the world's oil resources have become increasingly scarce, and the problem of heavy and inferior oil resources has become more and more obvious. At the same time, the market's demand for light oil has continued to increase and people's awareness of environmental protection has continued to increase. Engine exhaust emission requirements are more stringent, and various fuel standards require more stringent S and N content. How to process the middle distillate with high impurity content such as sulfur and nitrogen into products that meet the requirements of environmental protection is an important problem faced by every refinery. In this realistic environment, heavy oil hydrogenati...

Claims

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Application Information

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IPC IPC(8): B01J31/34C10G49/04C10G49/16
CPCB01J23/881B01J37/02C10G49/04
Inventor 李苏安邓清宇王坤朋
Owner CATECH TECH
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