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Method for synthesizing decalin

A synthesis method and decalin technology, which are applied in chemical instruments and methods, hydrogenation to hydrocarbons, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as high price and difficulty, and achieve low metal content, The effect of high naphthalene conversion

Inactive Publication Date: 2009-12-16
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Noble metal catalysts have very high hydrogenation activity and can usually deeply hydrogenate naphthalene, but they are expensive; non-noble metal catalysts such as nickel can easily hydrogenate naphthalene to tetrahydronaphthalene, but it is difficult to continue hydrogenation of tetrahydronaphthalene to decahydronaphthalene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] After fully dissolving nickel acetate in water, add γ-Al according to the metal content of 4% 2 o 3 After 5 hours, the clear liquid was poured out and dried at 150°C for 8 hours to obtain a catalyst precursor; the catalyst precursor was reduced at 450°C for 4 hours at a hydrogen flow rate of 30mL / min to obtain Ni / γ-Al with a nickel content of 4%. 2 o 3 Catalyst, the diameter of nickel metal particles is about 2-3nm. Ni / γ-Al 2 o 3 The catalyst is used under the protection of reducing gas for standby use. In a 0.1L high-pressure stirred reactor, add naphthalene to the solvent cyclohexane mass concentration ratio of 0.09 solution 40mL and nickel content of 4% catalyst 1.5g, at a reaction temperature of 180 ° C, a reaction pressure of 4MPa, a stirring speed of 750rpm conditions , the liquid mass space velocity is 11.0h -1 , Reaction 2h. The conversion rate of the hydrogenation reaction of naphthalene reaches 100%, and the yield of decahydronaphthalene reaches 99%.

Embodiment 2

[0025] The preparation of catalyst is the same as in Example 1. In a 0.1L high-pressure stirred reactor, add naphthalene to the solvent cyclohexane mass concentration ratio of 0.14 solution 40mL and a nickel content of 4% catalyst 1.5g, at a reaction temperature of 180 ° C, a reaction pressure of 4MPa, a stirring speed of 750rpm conditions , the liquid mass space velocity is 9.5h -1 , Reaction 2.5h. The conversion rate of the hydrogenation reaction of naphthalene reaches 100%, and the yield of decahydronaphthalene reaches 99%.

Embodiment 3

[0027] The preparation of catalyst is the same as in Example 1. In a 0.1L high-pressure stirred reactor, add the mass concentration ratio of naphthalene to the solvent cyclohexane: 40mL of a solution of 0.09 and 1.5g of a catalyst with a nickel content of 6.5%, the reaction temperature is 150°C, the reaction pressure is 3MPa, and the stirring speed is 650rpm. , the liquid mass space velocity is 11.0h -1 , Reaction 2h. The conversion rate of the hydrogenation reaction of naphthalene reaches 100%, and the yield of decahydronaphthalene reaches 98%.

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Abstract

The invention provides a method for synthesizing decalin, and relates to a method for synthesizing a compound. The invention provides the method for synthesizing the decalin from naphthalene in one step by using a load type catalyst taking nano metal with low content and small size as an active phase and under the conditions of low reaction temperature and pressure. The method comprises the following steps of: mixing the naphthalene and cyclohexane, and placing the mixture in a high pressure autoclave; adding a catalyst in the high pressure autoclave; and discharging air in the high pressure autoclave, stabilizing the pressure of hydrogen gas in the high pressure autoclave to between 2 and 5MPa for reaction, and obtaining the decalin. The conversion rate of the naphthalene is 100 percent, and the maximum yield of the decalin is 99 percent. The method for preparing the catalyst of Ni / gamma-Al2O3 comprises the following steps of: dissolving metallic salt of nickel in water, adding gamma-Al2O3 in the mixed solution, pouring clear solution out, and drying the clear solution to obtain a precursor of the catalyst; and reducing the precursor of the catalyst.

Description

technical field [0001] The present invention relates to a synthetic method of a compound. Background technique [0002] Decalin is a suitable solvent for the "dry spinning process" of ultra-high molecular weight polyethylene. In addition to being used as a solvent, it can also be used as the best dehydrogenation and cracking "endothermic fuel" for hypersonic aircraft and as a fuel cell for automobiles Excellent hydrogen storage medium. Some foreign companies have already produced decahydronaphthalene products, such as Chemos GmbH in Europe, Affllied Company (DegussaAG) in Germany, DuPont in the United States, Dow Chemical Ltd, Sigma-AldriCh, etc., which are expensive. [0003] The catalysts currently used for the hydrogenation of naphthalene to decahydronaphthalene mainly include nickel, molybdenum, tungsten, palladium, platinum, rhodium, ruthenium and iridium. Noble metal catalysts have very high hydrogenation activity and can usually deeply hydrogenate naphthalene, but t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/50C07C5/10B01J23/755B01J37/18
Inventor 方维平李枫伊晓东郑进保王跃敏
Owner XIAMEN UNIV
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