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Method for preparing decalin based on the catalytic hydrogenation of tetralin at room temperature, and organic solvent

A room temperature, catalytic hydrogenation technology of tetralin, applied in the field of methods and organic solvents, can solve the problems of difficult controllable design and preparation, unsafe, high reaction temperature and pressure, and achieves a good green and environmentally friendly production process and good economy. and social benefits, the effect of mild reaction conditions

Active Publication Date: 2017-12-01
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high loading of Pt (2.8wt.%), metal Pt is relatively expensive, the catalyst cost is high, and the reaction temperature and pressure are high (100°C and 6MPa), high energy consumption, unsafe, and difficult to realize industrial application
[0003] In summary, the existing problems in the prior art are: the current method of catalytic hydrogenation of tetrahydronaphthalene to produce decahydronaphthalene, because the controllable design and preparation of multi-element metal (especially ternary) catalyst nanostructures is difficult, mu

Method used

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  • Method for preparing decalin based on the catalytic hydrogenation of tetralin at room temperature, and organic solvent
  • Method for preparing decalin based on the catalytic hydrogenation of tetralin at room temperature, and organic solvent
  • Method for preparing decalin based on the catalytic hydrogenation of tetralin at room temperature, and organic solvent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Synthesis of Rh / NiCo / CNTs catalyst:

[0039] 1. Weigh (0.45~3.6g) NiCl 2 ·6H 2 O and (0.45~3.6g) CoCl 2 ·6H 2 O, dissolved in (45-90mL) deionized water, stirred at room temperature to obtain a clear solution.

[0040] 2. Add (5~15mL) ethanol to the above NiCl 2 ·6H 2 O and CoCl 2 ·6H 2 O solution.

[0041] 3. Add (5-25mL) reducing agent solution (sodium borohydride, sodium hypophosphite, hydrazine hydrate, ascorbic acid, or polyols such as ethylene glycol).

[0042] 4. Add (0.45-2.5g) carbon nanotubes (activated carbon or carbon black).

[0043] 5. Heat the reaction solution to (100-200°C).

[0044] 6. Filter and wash several times with ethanol and water respectively.

[0045] 7. Vacuum dry and keep at 60°C for 6h.

[0046] 8. Weigh to get NiCo / CNTs nanomaterials, add to RhCl 3 In the solution, carry out in situ reduction, filter, wash, vacuum dry, and keep at 60°C for 6h.

[0047] 9. The catalyst is 99.999% N at a temperature of (600-900°C) 2 Medium calc...

Embodiment 2

[0051] In the high-pressure stirred tank reactor (MS-50-316L type, 50mL), add Ru / NiCo / CNTs catalyst 0.0500g successively, tetralin is 10.0mL; Pass into nitrogen (purity ≥ 99.999%) to remove the Air: feed hydrogen (purity ≥ 99.999%) to remove the nitrogen in the kettle, close the outlet valve, and then continuously feed hydrogen, when the reaction pressure is 4.5MPa. Start stirring at a stirring rate of 500r / min, and react at a constant temperature of 25°C for 11 hours. After the reaction stops, the remaining gas is discharged, and the product is obtained by centrifugation. The product composition is analyzed by gas chromatography. The reaction result is: decahydronaphthalene selectivity 100%, decalin The yield of naphthalene was 15%.

Embodiment 3

[0053] In the high-pressure stirred tank reactor (MS-50-316L type, 50mL), add Ru / NiCo / CNTs catalyst 0.1500g successively, tetralin is 10.0mL; Feed nitrogen (purity ≥ 99.999%) to remove the Air: feed hydrogen (purity ≥ 99.999%) to remove the nitrogen in the kettle, close the outlet valve, and then continuously feed hydrogen, when the reaction pressure is 4.5MPa. Start stirring at a stirring rate of 500r / min, and react at a constant temperature of 25°C for 13 hours. After the reaction stops, the remaining gas is discharged, and the product is obtained by centrifugation. The composition of the product is analyzed by gas chromatography. The reaction result is: selectivity of decalin 100%, decahydro The yield of naphthalene was 65%. In addition, the catalyst was reused 10 times without any decrease in its selectivity and activity.

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Abstract

The invention belongs to the technical field of industrial catalysis of petrochemical industry, and discloses a method for preparing decalin based on the catalytic hydrogenation of tetralin at room temperature, and an organic solvent. The method comprises the following steps: using carbon nanotube-CNTs (activated carbon-AC or carbon black-C) as a carrier to prepare a ternary metal-loaded catalyst (denoted M1/M2M3/CNTs) loaded on M1M2 bimetallic nanoparticles with 0.4-6% Rh (Ir, Pt, Pd, Au or Ru) as nanoscale island, wherein M1 is equal to Rh, Ir, Pt, Pd, Au or Ru; M2 is equal to Ni, Fe, Co or Cu; M3 is equal to Ni, Fe, Co or Cu. The M1/M2M3/CNTs ternary metal-loaded catalyst provided by the invention has tremendous industrialization prospects with 100% decalin selectivity and yield, the adopted catalyst has the advantages of low loading capacity, simple preparation, low cost and good stability, and can be reused for many times.

Description

technical field [0001] The invention belongs to the technical field of petrochemical industrial catalysis, and in particular relates to a method for preparing decahydronaphthalene based on tetrahydronaphthalene catalytic hydrogenation at room temperature and an organic solvent. Background technique [0002] Aromatics or naphthalene is an important chemical raw material and platform compound, and its important product extension is aromatic ring hydrogenation products. Such as tetrahydronaphthalene (or naphthalene) catalytic hydrogenation, the main products are tetrahydronaphthalene, octahydronaphthalene and decahydronaphthalene. Both tetrahydronaphthalene and decahydronaphthalene are widely used high-boiling organic solvents. They are mainly used as solvents for oils, resins, rubber, etc., and can also be used as paint removers, lubricants, dyes, pesticides, pharmaceuticals, and hydrogen storage in fuel cells. medium etc. At present, decahydronaphthalene, as a highly volati...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C5/10C07C13/50D01F6/04D01D1/02
CPCB01J23/892C07C5/10C07C13/50D01D1/02D01F6/04
Inventor 朱丽华郑拓张欢
Owner JIANGXI UNIV OF SCI & TECH
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