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Preparation method of vulcanized hydrogenation catalyst

A hydrogenation catalyst and vulcanization-type technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problem of poor interaction between active metal components and elemental sulfur, unfavorable active metal components Severe vulcanization reaction, active metal components are difficult to interact with each other, achieve broad market application prospects, reduce preparation costs, and concentrate the pore size distribution

Active Publication Date: 2018-05-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the catalyst prepared by way 1 contains elemental sulfur and the hydrogenation active metal component is added step by step, that is, the elemental sulfur and the carrier precursor auxiliary and auxiliary agent are mixed first, and then combined with the active metal component after a certain heat treatment. Therefore, elemental sulfur first interacts with the carrier material, and it is difficult to interact well with the active metal component, which is not conducive to the vulcanization reaction of the active metal component, thereby affecting the utilization rate of the active metal and reducing the catalyst activity; Mode 2 When preparing the catalyst, the active metal component is directly mixed with the carrier precursor, elemental sulfur, auxiliary agent, and forming aid, and there is also the problem that the interaction effect of the active metal component and the elemental sulfur is not good.

Method used

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  • Preparation method of vulcanized hydrogenation catalyst
  • Preparation method of vulcanized hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 1. Prepare Mo-Ni-P solution: first add 50ml of clean water to the preparation container, start the agitator, slowly add 57.2 g of molybdenum oxide, 22.4 g of basic nickel carbonate, and finally slowly add 1.27 g of phosphoric acid to avoid basic carbonic acid The salt is heated and decomposed to produce carbon dioxide bump. After adding the materials, cover tightly, then heat up to >100°C, and keep the temperature constant for 1-2 hours, until the molybdenum oxide and basic nickel carbonate are completely dissolved, and the Mo-Ni-P solution is prepared. Mo-Ni-P solution concentration is MoO 3 57.1g / 100ml; NiO 9.8g / 100ml; P4.0g / 100ml;

[0044] 2. Take 10.9 g of elemental sulfur, 2 g of kerosene, and 22 g of rapeseed oil and mix for 15 minutes; add 5 g of Mo-Ni type EPRES external presulfurization catalyst UDS-6 (Φ3.0), heat up to 100-120 ° C, and keep the temperature for 5-15 min Then, add 0.5 g of polyethyleneimine, add 64 ml of the above-mentioned Mo-Ni-P solution, a...

Embodiment 2

[0051] 1. First, add 25ml of clean water into the preparation container, start the mixer, slowly add 9.8g of basic cobalt carbonate, 14g of citric acid, then heat up to >100°C, keep the temperature for 10-20min, and naturally cool to room temperature to obtain Co- Citric acid solution, the concentration is CoO 14.5g / 100ml;

[0052] 2. Mix 15.6g of dimethyl disulfide, 2g of diesel oil, 22g of soybean oil, and 3g of glycerin for 5 minutes; add 5g of Co-Mo type EPRES external presulfurization catalyst FH-40B (Φ3.0), and heat up to 100-120 ℃, keep the temperature for 25min; then, add 5g of sodium dodecylbenzenesulfonate, add 65ml of the above-mentioned Co-citric acid solution, and keep the temperature at 120℃ for 25min. Then, cool and separate and remove the external presulfided catalyst FH-40B to obtain liquid mixture I;

[0053] 3. Take 50ml of water, add 4.6ml of concentrated nitric acid to dilute to obtain dilute nitric acid; then add 5g of citric acid and 4g of urea, and the...

Embodiment 3

[0060] 1. First add 25ml of clean water to the preparation container, start the agitator, slowly add 9.8g of basic cobalt carbonate, 14g of citric acid, then heat up to >100°C, keep the temperature for 10-20min, and naturally cool to room temperature, the solution volume is 35ml . A Co-citric acid solution was prepared. Add ammonium heptamolybdate 18.2g then, add ammoniacal liquor (0.94g / ml specific gravity) 50ml again, prepare Co-Mo citric acid solution concentration and be MoO 3 , 21.1g / 100ml; CoO, 3.90g / 100ml;

[0061] 2. Take 12.9 g of elemental sulfur, 2.2 g of white oil, and 24 g of lard and mix for 15 minutes; add 5.0 g of oxidized Co-Mo catalyst UDS-5 (Φ3.0), raise the temperature to 100-120 ° C, and keep the temperature for 5-15 minutes; Add 2.5 g each of dodecyltrimethylammonium bromide and coconut oil fatty acid diethanolamide, then add 66ml of the above-mentioned Co-Mo citric acid solution, and keep the temperature at 120°C for 25min, then cool and separate to re...

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Abstract

The invention discloses a preparation method of a vulcanized hydrogenation catalyst. The method comprises the steps as follows: (1) a vulcanizing agent, a vulcanizing aid, an emulsifier and additive particles are uniformly mixed, the mixture is subjected to a constant-temperature reaction, then, an aqueous solution containing hydrogenation active metal is added, the mixture reacts for 5-60 min, the additive particles are removed by separation, and a liquid mixture I is obtained; (2) a peptizing agent, water and urea are uniformly mixed and a liquid mixture II is obtained; (3) an aluminum source is added to an acidic aqueous solution for slurry making, the liquid mixtures I and II are added, and the slurry is mixed uniformly; (4) the slurry in the step (3) is subjected to quick evaporativeconcentration to form concentrated slurry, slow drying treatment is performed, and a semi-dried material is obtained; (5) the semi-dried material obtained in the step (3) is ground, subjected to extrusion molding and roasting, and the vulcanized hydrogenation catalyst is obtained. The catalyst preparation and vulcanizing processes are completed simultaneously, and the catalyst has uniform pore diameter distribution, is simple to prepare and has wider market application prospects.

Description

technical field [0001] The invention relates to a preparation method of a sulfurized hydrogenation catalyst. Background technique [0002] Hydrofining, hydrotreating, hydrocracking and other oil refining catalytic hydrogenation production processes are environmentally friendly oil refining production processes, which can be widely used in the production of clean petroleum products such as gasoline, kerosene, diesel oil, lubricating oil, and paraffin. With the continuous upgrading of product quality, increasingly stringent environmental protection regulations, and increasingly inferior and heavy crude oil, hydrogenation technology has been widely valued and applied all over the world. The processing capacity of hydrogenation units in my country's oil refineries continues to grow, and the demand for hydrogenation catalysts is increasing year by year, and most of these catalysts can only obtain better performance after sulfidation. The presulfidation of catalysts (conversion o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188B01J27/19B01J35/10C10G45/08
CPCC10G45/08B01J27/188B01J27/19C10G2300/202B01J35/635B01J35/633B01J35/647B01J35/615
Inventor 高玉兰方向晨彭绍忠徐黎明吕振辉张学辉佟佳王继峰
Owner CHINA PETROLEUM & CHEM CORP
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