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Method for removing sulfide in simulated oil through oxidation by using transition metal tungstate as catalyst

A transition metal and tungstate technology, which is applied in the refining of oxygen-containing compounds, etc., can solve the problems of limited application and difficult recovery, and achieve the effects of easy recovery, low cost and simple process

Inactive Publication Date: 2013-10-02
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above Na 2 WO 4 As an oxidative desulfurization catalyst, it is difficult to recover after the reaction, and these shortcomings greatly limit its application in industry

Method used

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  • Method for removing sulfide in simulated oil through oxidation by using transition metal tungstate as catalyst
  • Method for removing sulfide in simulated oil through oxidation by using transition metal tungstate as catalyst

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Experimental program
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Embodiment 1

[0021] Transition metal tungstates include the following: CuWO 4 , NiWO 4 , CoWO 4 , MnWO 4 , 4 kinds of tungstate reference [U.M. García-Pérez, A. Martínez-de la Cruz, J. Peral. Transition metal tungstates synthesized by co-precipitation method: Basic photocatalytic properties[J]. Electrochimica Acta, 2012, 81: 227-232].

[0022] A. Synthesis of transition metal nickel tungstate.

[0023] The specific preparation process is as follows: Weigh a certain mass of transition metal nickel nitrate, dissolve it in water, add sodium tungstate, stir at room temperature for 3 hours, collect the product and wash it with water and dry it at 70°C for 6 hours, and then put the product in a muffle furnace for 500 Calcined at ℃ for 4h.

[0024] B. Simulate oil desulfurization.

[0025] Add 0.01g of nickel tungstate to 10 mL of simulated oil with a sulfur content of 500 μg / g prepared by a certain amount of dibenzothiophene (DBT), add 0.2mL of H 2 o 2 and 0.01g of cetyltrimethylammon...

Embodiment 2

[0029] A. Synthesis of transition metal cobalt tungstate.

[0030] The specific preparation process is as follows: Weigh a certain mass of transition metal cobalt nitrate salt, dissolve it in water, add sodium tungstate, stir at room temperature for 2 hours, collect the product and wash it with water and dry it at 75°C for 6 hours, and then put the product in the muffle furnace Calcined at 500°C for 4h.

[0031] B. Simulate oil desulfurization.

[0032] Add 0.01g cobalt tungstate to 10 mL simulated oil with a sulfur content of 500 μg / g prepared by a certain amount of dibenzothiophene (DBT), add 0.2 mL H 2 o 2 , after reacting at 30°C for 30 min in a constant temperature water bath equipped with magnetic stirring, the reaction mixture was cooled to room temperature, and the layers were separated in a separatory funnel to separate the oil phase. Add 5 mL of N-N-dimethylformamide and continue to stir for 10 min, statically separate layers, separate the oil phase, measure the ...

Embodiment 3

[0036] Add 0.01g manganese tungstate to 10 mL simulated oil with a sulfur content of 500 μg / g prepared by a certain amount of dibenzothiophene (DBT), add 0.2 mL H 2 o 2 , after reacting at 30°C for 30 min in a constant temperature water bath equipped with magnetic stirring, the reaction mixture was cooled to room temperature, and the layers were separated in a separatory funnel to separate the oil phase. Add 5 mL of N-N-dimethylformamide and continue to stir for 10 min, statically separate layers, separate the oil phase, measure the sulfur content and calculate the desulfurization rate to be 89%.

[0037] The synthesis steps and recovery steps of the transition metal manganese tungstate are the same as above.

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Abstract

The invention belongs to the field of vehicle fuel desulfurization realized through catalytic oxidation and particularly relates to a method for removing a sulfide in simulated oil through oxidation by using transition metal tungstate as a catalyst. The method can be implemented according to the following steps of: (1) weighting the transition metal tungstate, adding water to dissolve the transition metal tungstate, adding sodium tungstate and stirring at room temperature; collecting a product, drying the product after the product is washed, and then, calcining the product to obtain the transition metal tungstate; (2) adding the tungstate into the simulated oil, adding an oxidizing agent and cetyltrimethylammonium bromide, cooling a reaction mixture to the room temperature, and separating out an oil phase, wherein the tungstate is synthesized in the step (1), further adding N-N-dimethyl formamide and stirring, separating out the oil phase, measuring the sulphur content and calculating the desulfurization degree; and (3) recovering a tungstate catalyst, drying and washing to remove the surface sulfide, and drying the tungstate catalyst for repeated use. The method is simple in process, low in cost and high in desulfurization degree; the transition metal tungstate is easy to recover after reaction and can be repeatedly used after regeneration.

Description

technical field [0001] The invention belongs to the field of catalytic oxidation desulfurization of fuel for vehicles, and in particular relates to a method for oxidizing and removing sulfide in simulated oil by using transition metal tungstate as a catalyst. Background technique [0002] With the rapid development of the automobile industry, the pollution of sulfur compounds produced by the combustion of vehicle fuels is becoming more and more serious. Countries and regions around the world have successively formulated strict standards for the sulfur content of gasoline and diesel [1]. In industry, hydrodesulfurization (HDS) is usually used to remove sulfide in gasoline and diesel, but for thiophene and its derivatives, due to the steric hindrance effect, the desulfurization effect is poor. In order to achieve the purpose of deep desulfurization, the reaction conditions must be changed. and catalysts put forward higher requirements, which in turn leads to an increase in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G27/12
Inventor 赵荣祥李秀萍
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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