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Organic molybdenum salt composition and a preparation method thereof

A technology of organic molybdenum and its composition, which is applied in the field of molybdenum-containing organic matter and its preparation, can solve the problems of not being able to meet the requirements of energy conservation and environmental protection, high addition of molybdenum naphthenate, low content of molybdenum naphthenate, etc., and achieve no special pollution waste emissions, high conversion rate, and environmentally friendly production routes

Inactive Publication Date: 2018-04-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing molybdenum-containing organic compounds are mainly used in the lubrication field, but most of the molybdenum-containing organic compounds that have been developed have poor oil solubility, corrosion problems and environmental protection problems due to the presence of compounds such as sulfur and phosphorus.
CN101165141A discloses a preparation process of molybdenum naphthenate as a catalyst for coal-to-liquids, which can be produced under milder conditions, but the content of molybdenum naphthenate prepared by this process is low, and molybdenum naphthenate The amount added is higher
CN92102723A discloses a preparation process of molybdenum naphthenate and its molybdenum-sulfur antiwear agent. The process is to react naphthenic acid with sodium hydroxide to form sodium naphthenate solution, and react molybdenum trioxide with sodium hydroxide to form molybdenum molybdenum Sodium molybdate, then dilute and stir sodium molybdate and sodium naphthenate under the action of water, petroleum ether, and benzene, add hydrochloric acid dropwise in the process to adjust the pH value, and then process to obtain molybdenum naphthenate. In this preparation process, a large amount of Alkaline and acid cannot meet the increasingly stringent energy saving and environmental protection requirements
The precursor is then deposited on an oxide support suitable for the process it is used in, but the precursor contains sulfur and is mainly used for fixed bed hydrogenation, not suitable for slurry bed hydrogenation process

Method used

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preparation example Construction

[0020] The preparation method of above-mentioned organic molybdenum salt composition, comprises the following steps:

[0021] (1) The hexavalent molybdenum source compound is dissolved and dispersed in a solvent, and the catalytic effect of adding an inorganic acid is added. The mass ratio of the inorganic acid catalyst to the hexavalent molybdenum source is (0.05~0.2):1, and C1~ C5 organic acid, described solvent is benzene, toluene, water, ethanol or sherwood oil;

[0022] (2) After the reaction, the solvent phase is removed to obtain an intermediate product;

[0023] (3) Mixing and reacting the intermediate product with C6-C16 organic acid or C6-C16 ester;

[0024] (4) After the mixing is completed, the mixture is reacted at a temperature of 50-350° C. under reducing atmosphere conditions, and then the product is collected after vacuum distillation to obtain an organic molybdenum salt composition.

[0025] In the preparation method of the organic molybdenum salt compositi...

Embodiment 1

[0038] Molybdenum trioxide and toluene were dispersed in the flask according to the mass ratio of 1:24, purged with inert gas, and succinic acid was added to react at a temperature of 60°C for 6 hours, and the molar ratio of the amount of succinic acid to molybdenum trioxide was 1: 3; After the reaction is finished, the solvent is separated to obtain an intermediate product. The molar ratio of molybdenum trioxide and heptanoic acid is 1:6, the mixing temperature is 60°C, and the mixing time is 30 minutes. After the mixing is completed, the reaction is carried out for 10 hours at a temperature of 280° C. under a hydrogen atmosphere and a reaction pressure of 0.2 MPa, and the product is obtained after the reaction is completed. The solubility of the obtained product is shown in Table 1. The metal content analysis of the product was carried out, and the analysis method adopted was inductively coupled plasma emission spectrometry (GB / T 17476). The metal valence state analysis af...

Embodiment 2

[0040] Molybdenum trioxide and toluene were dispersed in the flask according to the mass ratio equal to 1:15, purged with inert gas, and added formic acid at a temperature of 80°C for 6 hours, the molar ratio of the amount of formic acid to molybdenum trioxide was 1:5; the reaction ended Afterwards, the solvent was separated to obtain an intermediate product. Mix according to the molar ratio of molybdenum trioxide and n-octanoic acid of 1:4, the mixing temperature is 80°C, and the mixing time is 40 minutes. After the mixing is completed, the temperature is 200° C. under hydrogen atmosphere, the reaction pressure is 1 MPa, and the reaction time is 15 hours. After the reaction is completed, the product is obtained. The solubility of the obtained product is shown in Table 1. The metal content analysis of the product was carried out, and the analysis method adopted was inductively coupled plasma emission spectrometry (GB / T 17476). The metal valence state analysis after sample tr...

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Abstract

The invention relates to organic molybdenum salt composition and a preparation method thereof. The organic molybdenum salt composition contains a molybdenum ion and C1-C16 organic anions bound with the molybdenum ion, wherein the organic anions contain oxygen atoms, and valence states of molybdenum in the molybdenum ion is +3, +4 and +5 in a molar ratio of (0.1-20.0): (15.0-45.0): (40.0-75. 0). The provided organic molybdenum salt has high metal content and good solubility in oil phase, and can be used as a catalyst precursor for slurry bed residual oil hydrogenation, conversion rate in the reaction process is high, the product property is stable, and a filtration step is needless. The provided organic molybdenum salt composition is low in synthesis cost, the production route is environmentally friendly, and no pollutant is discharged in the production process.

Description

technical field [0001] The invention relates to a molybdenum-containing organic compound and a preparation method thereof, more specifically, an organic molybdenum salt composition and a preparation method thereof. Background technique [0002] Global oil resources are becoming increasingly heavy and inferior. In order to meet the needs of national economic growth and people's living needs, deep processing of heavy oil and improvement of resource utilization have become increasingly concerned issues. Heavy oil processing technology is divided into two categories: decarburization and hydrogenation. In order to further increase the yield of light oil, hydrogenation technology plays an increasingly important role in the field of heavy oil processing. The slurry bed residual oil hydrogenation process uses a homogeneous catalyst, the catalyst precursor is dispersed in the residual oil, and then the hydrogenation reaction is carried out directly through the reactor. Hydroprocessi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C55/10C07C53/126C07C53/06B01J31/04B01J37/20C10G47/02C10M129/32C10M129/34C10M129/40C10N30/06C10N10/12
CPCB01J31/04B01J37/20C07C51/412C07C53/06C07C53/126C07C55/10C10G47/02C10M129/32C10M129/34C10M129/40C10M2207/122C10M2207/123C10M2207/126C10N2010/12C10N2030/06
Inventor 王红王子军王翠红佘玉成申海平
Owner CHINA PETROLEUM & CHEM CORP