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Method for synthesizing decalin

A decalin and catalyst technology is applied in the field of chemical engineering to achieve the effects of low metal content, production cost saving and effective utilization

Inactive Publication Date: 2012-01-18
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the current synthetic method, there are still some deficiencies. Therefore, further optimization of the process conditions for the synthesis of decahydronaphthalene is of great significance for industrialized large-scale production of decahydronaphthalene.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take by weighing 0.1424g purity and be 59% palladium chloride, and it is fully dissolved in the dilute hydrochloric acid of 0.6% in mass concentration, add gamma-Al 2 o 3 Spherical particles 10g, moved to a rotary evaporator, set the water temperature to 50°C, vacuumed and evaporated until the water was evaporated to dryness, and obtained the catalyst precursor; put the catalyst precursor into the muffle furnace and raised the temperature to 400°C for 5h, and then 25ml / min, hydrogen flow rate 5ml / min, reduction at 250℃ for 4h, that is, Pd / γ-Al with a loading capacity of 0.5% is obtained 2 o 3 catalyst.

[0021] The prepared catalyst is loaded into the fixed bed reaction tube, and the upper and lower sides are filled with 20-40 mesh quartz sand. Using cyclohexane as a solvent, the raw materials were prepared according to the mass ratio of naphthalene:cyclohexane=1:9. The raw materials enter the fixed-bed reactor through the high-pressure infusion pump for reaction. ...

Embodiment 2

[0023] Weigh the palladium nitrate of 0.0650g, and it is fully dissolved in the dilute nitric acid that mass concentration is 20%, add gamma-Al 2 o 3 Spherical particles 10g, moved to a rotary evaporator, set the water temperature to 45°C, vacuumed and evaporated until the water was evaporated to dryness, and obtained the catalyst precursor; put the catalyst precursor into the muffle furnace and heated it to 500°C for 4 hours, and then 26ml / min, hydrogen flow rate 4ml / min, 300℃ reduction for 3h, that is, Pd / γ-Al with a loading capacity of 0.3% 2 o 3 catalyst.

[0024] The prepared catalyst is loaded into the fixed bed reaction tube, and the upper and lower sides are filled with 20-40 mesh quartz sand. Using cyclohexane as a solvent, the raw materials were prepared according to the mass ratio of naphthalene:cyclohexane=1:7. The raw materials enter the fixed-bed reactor through the high-pressure infusion pump for reaction. At a reaction temperature of 200°C, a reaction pres...

Embodiment 3

[0026] Take by weighing 0.1977g purity to be the palladium chloride of 59%, and it is fully dissolved in the dilute hydrochloric acid that mass concentration is 4%, add gamma-Al 2 o 3 Spherical particles 10g, moved to a rotary evaporator, set the water temperature to 60°C, evaporated in a vacuum until the water was evaporated to dryness, and obtained the catalyst precursor; put the catalyst precursor into the muffle furnace and raised the temperature to 450°C for 5 hours, and then 24ml / min, hydrogen flow rate 6ml / min, 330℃ reduction for 3h, that is, Pd / γ-Al with a loading capacity of 0.7% was obtained 2 o 3 catalyst.

[0027] The prepared catalyst is loaded into the fixed bed reaction tube, and the upper and lower sides are filled with 20-40 mesh quartz sand. Using n-heptane as a solvent, the raw materials were prepared according to the mass ratio of naphthalene:n-heptane=1:10. The raw materials enter the fixed-bed reactor through the high-pressure infusion pump for reacti...

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Abstract

The invention relates to a method for synthesizing decalin, which comprises the following specific steps: naphthalene is dissolved in an organic solvent to be prepared into a reaction raw material, then a prepared catalyst Pd / gamma-Al2O3 is arranged in a reaction tube of a fixed bed reactor, the upper part and the lower part of the reaction tube are filled with quartz sand, the raw material enters the fixed bed reactor through a high-pressure infusion pump for reaction so as to obtain the decalin, wherein the reaction temperature is controlled to be 100-280 DEG C, the reaction pressure is 1.5-4.0Mpa, the liquid hour mass space velocity is 0.5-2.0h-1, and the hydrogen oil ratio is 80-1000. The maximum conversion rate of the naphthalene reaches 99.92%, and the yield of the decalin reaches 99.36%.

Description

technical field [0001] The invention relates to a method for synthesizing decahydronaphthalene by catalytic hydrogenation of naphthalene in a fixed-bed reactor at relatively low temperature and pressure, and belongs to the technical field of chemical engineering. Background technique [0002] Decalin is an excellent high-boiling organic solvent that can dissolve certain polymer compounds, such as it can be used as a solvent for ultra-high molecular weight polyethylene. It can also be used as a solvent for paints, used to extract fats and waxes, and used in the manufacture of shoe polish and floor wax instead of turpentine. Since naphthalene can be catalytically hydrogenated to synthesize decahydronaphthalene, and the generated decahydronaphthalene can be catalytically hydrogenated under suitable conditions to release pure hydrogen, so this feature can be used as a new type of hydrogen storage material. [0003] In the patent of CN 1546442A, tetrahydronaphthalene is used as ...

Claims

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Application Information

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IPC IPC(8): C07C13/50C07C5/10B01J23/44
Inventor 周志伟孔冀武文良任晓乾李超
Owner NANJING UNIV OF TECH
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