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Preparation method for supported Mo-based oxidation and desulfurization catalyst

A technology of oxidative desulfurization and catalyst, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, molecular sieve catalysts, etc., can solve problems such as loss of oil products, difficulty in completely separating oil from water, and environmental pollution. To achieve the effect of enhancing the activity

Inactive Publication Date: 2011-12-28
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology improves on existing methods used for reducing carbon dioxides from fossil fuel combustion emissions through use of molten salts containing alkali metals such as sodium (Na) or potassium (K). These processes involve reactants made up mostly of water solubles called cobalt(III), which are mixed together at high temperatures. By adding these chemicals during the treatment step, they help break down harmful pollutants like nitrogen compounds found in exhaust gases produced after burning them.

Problems solved by technology

Technologies described involve combining different types of chemical agents like hydrotreating/hydrocracking techniques together with oxidizing processes like oxidoreduclotriphosphorus (OPHT), nitrothia cyanate(NTC)-dispersive solvent method, liquid scavengers containing ammonium salts, metal chelates, ion exchange resin columns, and activated carbon layers on supports made of porous materials called mesoporous silica. These technics aim to combine various chemistry principles while minimizing wastage and production expenses associated with conventional methods involving multiple phases.

Method used

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  • Preparation method for supported Mo-based oxidation and desulfurization catalyst
  • Preparation method for supported Mo-based oxidation and desulfurization catalyst
  • Preparation method for supported Mo-based oxidation and desulfurization catalyst

Examples

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Effect test

Embodiment 1

[0020] Preparation of citric acid modified MoO 3 / SiO 2 catalyst

[0021] Firstly, supported MoO was prepared by isometric impregnation method 3 / SiO 2 Catalyst: Weigh 0.920g of ammonium molybdate and dissolve it in 9g of deionized water to make a solution, add dropwise to 3g of white carbon black, stir evenly, let stand at room temperature for 12h, dry at 120°C for 4h, and heat up at a rate of 2°C / min to 500°C, after calcination for 5h, SiO was prepared 2 Loaded MoO 3 Catalyst, denoted as MoO 3 / SiO 2 , where MoO 3 The loading capacity is 20% by mass fraction.

[0022] Then weigh 0.3g of citric acid and dissolve it in 1g of deionized water to form a solution, and add it dropwise to 1g of prepared MoO 3 / SiO 2 In the sample, stir evenly, stand at room temperature for 4 hours, and dry at 100°C for 2 hours. Then, the catalyst was subjected to a temperature-programmed heat treatment under a nitrogen atmosphere: at room temperature, the temperature was raised to 120°C a...

Embodiment 2

[0024] Preparation of oxalic acid modified MoO 3 / SiO 2 Catalyst: Weigh 0.2g of oxalic acid and dissolve it in 1g of deionized water to make a solution, add it dropwise to 1g of prepared MoO 3 / SiO 2 In the sample, stir evenly, stand at room temperature for 4 hours, and dry at 100°C for 2 hours. Under a nitrogen atmosphere, the catalyst was subjected to temperature-programmed heat treatment: at room temperature, the temperature was raised to 150°C at a rate of 2°C / min, and kept for 1 hour, then raised to 250°C at a rate of 2°C / min, kept for 1 hour, and then heated at a rate of 2°C / min. Raise the temperature to 300°C at a rate of min and keep it for 1 hour to prepare a catalyst, which is denoted as OA-MoO 3 / SiO 2, the loading amount of oxalic acid is 20% by mass fraction. Depend on image 3 It can be seen that in OA-MoO 3 / SiO 2 Simultaneously observed Mo on the surface 6+ and low-valence Mo 5+ species.

Embodiment 3

[0026] The catalyst in the embodiment 1 or 2 of 0.2g is loaded in the internal diameter 8mm fixed-bed reactor, with the toluene solution of the dibenzothiophene of mass fraction 0.2% as simulated oil product, with hydroxycumene peroxide as oxidant Continuous oxidative desulfurization reaction. Other reaction conditions are: O / S molar ratio = 4, normal pressure, reaction temperature 50°C, WHSV = 32h -1 . Depend on Figure 4 It can be seen that the oxidative desulfurization activity of the catalyst modified by citric acid or oxalic acid is higher than that of MoO 3 / SiO 2 There is a significant improvement.

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Abstract

The invention discloses a preparation method for a supported Mo-based oxidation desulfurization catalyst, and belongs to the technical fields of coal processing, petroleum processing and petrochemical processing, and relates to a preparation method for a solid catalyst for oxidative removal of distillate oil and sulphide-containing thiophene aromatic heterocyclic compounds in the chemical materials. The method is characterized by: loading an organic acid on a porous carrier-supported Mo-based oxide catalyst, then drying at a temperature of 70-120 DEG C; heating to the temperature of 100-180 DEG C in the protection of inert gas, and holding for 1-5 hours, wherein the heating rate is 1-10 DEG C per minute; then heating to the temperature of 200-260 DEG C and holding for 1-5 hours, wherein the heating rate is 1-10 DEG C per minute; then heating to the temperature of 300-340 DEG C and holding for 1-5 hours, wherein the heating rate is 1-10 DEG C per minute to prepare the catalyst. The mixture comprising Mo<6+> and low valence state Mo<5+> is loaded on the surface of the catalyst. With the present invention, the oxidation activity and the desulfurization activity of the supported Mo-based catalyst provided by the present invention can be significantly improved, and a wide application prospect in the field of deep desulfurization is provided.

Description

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Claims

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Application Information

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Owner DALIAN UNIV OF TECH
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