Method for producing decalin through crude naphthalene hydrodesulfurization

A technology for hydrodesulfurization and decalin, which is applied in chemical instruments and methods, hydrogenation to hydrocarbons, hydrocarbons, etc., can solve the problems of short service life of catalysts, increased production costs, and high content of precious metals in hydrogenation catalysts, and can prolong the life of the catalyst. Service life, low operating pressure, elimination of activity inhibition and poisoning effects

Active Publication Date: 2017-04-19
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the noble metal content in the hydrogenation catalyst in the second stage of the method is high, which greatly increases the production cost
At the same time, the firs

Method used

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  • Method for producing decalin through crude naphthalene hydrodesulfurization

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Experimental program
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Effect test

Embodiment 1

[0034] Using cyclohexane as a solvent, the raw materials are configured according to the mass ratio of industrial naphthalene:cyclohexane=10:90.

[0035] The loading capacity of the first-stage hydrogenation catalyst is 100ml, the catalyst is a Ni-Mo catalyst, and the carrier is Al 2 o 3 , based on the weight of the catalyst, where the content of NiO is 8%, MO 3 The content is 16%. The catalyst needs to be pre-sulfided in the reactor before use, using carbon disulfide / cyclohexane with a volume content of 2% as the vulcanizing agent, and the vulcanized liquid space velocity is 1h -1 , the gas-liquid volume ratio is 600:1. After the catalyst is vulcanized at 240°C for 24 hours, continue to vulcanize at 300°C for 6 hours, use lead acetate to check whether the vulcanization is complete, and stop the vulcanization after the vulcanization is complete. The first hydrogenation reaction temperature is 280°C, the reaction pressure is 4MPa, and the liquid space velocity is 1h -1 , T...

Embodiment 2

[0040] This implementation operates according to Example 1, but there are the following differences:

[0041] Using cyclohexane as a solvent, configure raw materials according to the mass ratio of industrial naphthalene: cyclohexane=10:90;

[0042] The first-stage hydrogenation catalyst component and loading are the same as those in Example 1, and it needs to be pre-sulfurized in the reactor before use, using dimethyl disulfide / cyclohexane with a volume content of 2% as the vulcanizing agent, and the vulcanized liquid space velocity for 1h -1 , the gas-liquid volume ratio is 600:1; after the catalyst is vulcanized at 240°C for 24 hours, continue to vulcanize at 300°C for 6 hours, use lead acetate to detect whether the vulcanization is complete, and stop vulcanization after the vulcanization is complete. The first hydrogenation reaction temperature is 300°C, the reaction pressure is 4MPa, and the liquid space velocity is 2h -1 , the gas-liquid volume ratio is 600:1;

[0043]...

Embodiment 3

[0047] This implementation operates according to Example 1, but there are the following differences:

[0048] With n-heptane as solvent, configure raw materials according to mass ratio industrial naphthalene: n-heptane=10:90;

[0049] The one-stage hydrogenation catalyst component and loading are the same as in Example 1, and it needs to be pre-sulfurized in the reactor before use, using dimethyl disulfide / cyclohexane with a volume content of 2% as the vulcanizing agent, and the vulcanized liquid space velocity for 1h -1 , the gas-liquid volume ratio is 600:1. After the catalyst is vulcanized at 240°C for 48 hours, use lead acetate to detect whether the vulcanization is complete, and stop the vulcanization after the vulcanization is complete. The first hydrogenation reaction temperature is 300°C, the reaction pressure is 6MPa, and the liquid space velocity is 2.5h -1 , the gas-liquid volume ratio is 400:1;

[0050] The washing tower uses sodium carbonate solution, the oper...

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Abstract

The invention provides a method for producing decalin through crude naphthalene hydrodesulfurization, and belongs to the technical field of environmental protection and energy. A high-purity decalin product is obtained through the following processes in order: dissolving through a dissolving tower, the first-stage hydrogenation, washing, fine desulfurization, the secondary hydrogenation and rectification. The fine desulfurization process is added between the washing and the secondary hydrogenation to remove the sulfur in the first-stage hydrogenation product, so that the content of the sulfur is reduced to 1ppm and lower, the active inhibition and poison to the secondary hydrogenation catalyst are relieved, the service life of the catalyst is prolonged, and the production cost is lowered. A nickel-based catalyst is used in the secondary hydrogenation so as to further lower the production cost. The crude naphthalene is used as the raw material, the raw material purity requirement is low, and the application scope is wide; by use of the two-stage type hydrogenation, the operation pressure is low, the decalin selectivity is greater than 99%, the total yield of the decalin is greater than 95%, and the product purity is greater than 99%.

Description

technical field [0001] The invention belongs to the technical field of environmental protection and energy, and specifically relates to a method for producing decalin by hydrodesulfurization of industrial naphthalene. Background technique [0002] As an excellent organic solvent with high boiling point, decahydronaphthalene is the best solvent in the dry spinning process of producing polyethylene fiber, a solvent for ultra-high molecular weight polyethylene, and it is also essential to improve the thermal stability of aviation kerosene additive. At present, decahydronaphthalene is mainly synthesized by hydrogenation of naphthalene. [0003] The research on the preparation of decahydronaphthalene by hydrogenation of naphthalene was earlier, and it began in foreign countries as early as the 1920s and 1930s. At present, only a few foreign companies such as DegussaAG in Germany, Chemos GmbH in Europe, DuPont in the United States, Dow Chemical Ltd, and Sigma-Aldrich produce dec...

Claims

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Application Information

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IPC IPC(8): C07C5/11C07C5/10C07C7/00C07C7/148C07C13/48C07C13/50C07C1/32C07C15/073C07C15/02
CPCC07C1/322C07C1/323C07C5/10C07C5/11C07C7/005C07C7/1485C07C2521/04C07C2521/06C07C2521/08C07C2523/755C07C2523/883C07C13/48C07C13/50C07C15/073C07C15/02
Inventor 苏敏张新波张明胜向建安谭建冬
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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