Oil soluble molybdenum-based precursor of catalyst, preparation method and application thereof

A molybdenum-based catalyst and oil-soluble technology, applied in chemical instruments and methods, organic chemistry, hydrocarbon oil cracking, etc., can solve the problems of high production cost and low catalytic hydrogenation activity, and achieve short reaction time and high catalytic hydrogenation activity The effect of high and low production cost

Inactive Publication Date: 2014-08-13
CHINA UNIV OF PETROLEUM (EAST CHINA)
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Problems solved by technology

[0005] The invention proposes an oil-soluble molybdenum-based catalyst precursor and its preparation method and application, which solves the problem that the molybdenum-based catalyst precursor in the prior art needs to add a vulcanizing agent to convert it into a molybdenum sulfide active substance with catalytic activity, which leads to catalytic hydrogenation activity The problem of low and high production costs

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  • Oil soluble molybdenum-based precursor of catalyst, preparation method and application thereof
  • Oil soluble molybdenum-based precursor of catalyst, preparation method and application thereof
  • Oil soluble molybdenum-based precursor of catalyst, preparation method and application thereof

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preparation example Construction

[0040] A preparation method of an oil-soluble molybdenum-based catalyst precursor, comprising the following steps:

[0041] 1) Mix molybdenum source and water at a molar ratio of 1:10 to 2:1, react at 70 to 90°C for 30 to 240 minutes, cool to 30 to 50°C, add inorganic acid dropwise to make the solution neutral;

[0042] 2) According to the molar ratio of hydroxyl group in polycarbonate alcohol to phosphorus pentasulfide is 3:1~5:1, add polycarbonate alcohol into phosphorus pentasulfide, the addition temperature is 50~80℃, and the addition time is 5~15min. At a temperature of 70-100°C, react for 1-3 hours, and purge the hydrogen sulfide gas generated during the reaction with an inert gas;

[0043] 3) Add the product obtained in step 2) to the product obtained in step 1), and add an acidic cation exchange resin, the quality of the acidic cation exchange resin is 10-15% of the molybdenum mass in the molybdenum source, at 70-110 ° C, react 4~8h;

[0044] 4) Separating the produc...

Embodiment 1

[0053] Take 0.5mol MoO 3 and 1.2mol NaOH, add 5mol water, in a 70°C water bath, stir and reflux for 240min, cool to 40°C, add 0.75mol concentrated H 2 SO 4 , make the solution neutral, and obtain the molybdenum source compound; take 3.0 mol of n-butanol and isooctyl alcohol mixed solution into the dropping funnel, dropwise add 1.0 mol of P 2 S 5 In a round-bottomed flask, the dropping temperature is 80°C, and the dropping time is 5 minutes. After the dropping is completed, react at 80°C for 3 hours. During the reaction, the solution is magnetically stirred and nitrogen gas is introduced, and the hydrogen sulfide gas is continuously purged to remove the generated hydrogen sulfide gas. ; Filtration, filter out the unreacted P 2 S 5 , transfer the filtrate into the dropping funnel, and add it dropwise to the above-mentioned molybdenum source compound, add 4.8g of acidic cation ion exchange resin to the mixed solution, stir and reflux at 95°C for 4h; filter, stand still, separ...

Embodiment 2

[0056] Take 0.5mol Na 2 MoO 4 2H 2 O, add 0.25mol water, stir and reflux for 30min in a water bath at 80°C, cool to 30°C, add 0.5mol concentrated H 2 SO 4 , acidified to obtain the molybdenum source compound; get 4.5mol of isooctyl alcohol and add it to the dropping funnel, and dropwise dropwise add 1.5mol of P 2 S 5 In the round-bottomed flask, the dropping temperature is 50°C, and the dropping time is 10 minutes. After the dropping is completed, the temperature is 90°C, and the reaction is carried out for 2 hours. During the reaction, magnetic stirring is used, and nitrogen gas is continuously purged to remove Generated hydrogen sulfide gas; cooling, filtering, filtering out unreacted P 2 S 5 , move the filtrate into the dropping funnel, and add it dropwise to the above-mentioned molybdenum source compound, and add 6g of acidic cation exchange resin, the acidic cation exchange resin is a sodium-type cation-exchange resin that is treated with sulfuric acid to be a hydro...

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Abstract

The invention provides an oil soluble molybdenum-based precursor of a catalyst, a preparation method and application thereof, relating to the technical field of heavy oil hydrocracking catalysts and solving the problems of low catalytic hydrogenation activity and high cost of the existing catalysts. The preparation method for the precursor comprises the steps of (1) mixing a molybdenum source with water, reacting for 30-240 minutes at 70-90DEG C, and adding inorganic acid; (2) adding polycarbon alcohol into P2S5 in 5-15 minutes at 50-80DEG C, and reacting for 1-3 hours at 70-100DEG C; (3) adding the product of step (2) into the product of step (1), adding resin, and reacting for 4-8 hours at 70-110DEG C; (4) separating oil phase from the product of step (3) so as to obtain the target product. The precursor can form MoS2 active components through self sulfurization and in situ decomposition, is used in slurry reactor hydrocracking of poor heavy oil with high content of metal, carbon residue and sulfur, and can lower the yield of coke and keep a device to run for a long period.

Description

technical field [0001] The invention relates to the technical field of heavy oil hydrocracking catalysts in petroleum processing technology, in particular to an oil-soluble molybdenum-based catalyst precursor and its preparation method and application. Background technique [0002] Heavy oil slurry bed hydrocracking is a heavy oil hydrothermal cracking process under high hydrogen pressure and high temperature. A small amount of catalyst precursor is in full contact with raw material residue oil and hydrogen in the reactor, showing a full back-mixing state. The organomolybdenum catalyst precursor is dissolved in the raw material oil. The main function of the catalyst precursor is to self-sulfurize in the residue oil to form Molybdenum sulfide with hydrogen activity can annihilate the free radicals in the thermal cracking process of residual oil, inhibit condensation and reduce coke formation, so as to achieve a lower coke formation and a higher conversion rate in the entire h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F11/00B01J27/051C10G47/06C10G47/26
Inventor 邓文安李传张倩倩李庶峰文萍沐宝泉
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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