Method for catalyzing dimerization-hydrogenation reaction of alpha-pinene by using bifunctional microporous molecular sieve

A microporous molecular sieve and hydrogenation reaction technology, applied in molecular sieve catalysts, molecular sieves and base exchange compounds, chemical instruments and methods, etc., can solve difficult problems, lack of shape-selective properties of mesoporous catalytic materials, affecting low-temperature viscosity of oil products and Freezing point and other issues, to achieve good catalytic performance, easy to separate and reuse, high activity effect

Active Publication Date: 2021-06-18
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, only Pd-Al-MCM-41 is used to directly catalyze the dimerization-hydrogenation reaction of β-pinene with one-pot (Zhang S, XuC, Zhai G, et al.Bifunctional catalyst Pd-Al-MCM-41 for efficient dimerization -hydrogenation ofβ-pinene in one pot[J].RSC Advances,2017,7(75):47539-47546), although a higher yield of dimer was obtained, but due to the shape-selective properties of mesoporous catalytic materials The lack of oligomeric products also produces a large amount of deep oligomerization products. This part of the product with too high molecular weight may need cumbersome separation process to remove, or stay in the product, which will seriously affect the low temperature viscosity and freezing point of the oil.
In addition, it is more difficult to catalyze the dimerization-hydrogenation reaction of α-pinene with one-pot bifunctional catalyst, which has not been reported yet.

Method used

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  • Method for catalyzing dimerization-hydrogenation reaction of alpha-pinene by using bifunctional microporous molecular sieve
  • Method for catalyzing dimerization-hydrogenation reaction of alpha-pinene by using bifunctional microporous molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0016] SiO 2 :Na 2 O: Al 2 o 3 :TEAOH:H 2 O = 1: 0.064: 0.04: 0.43: 10.5 The proportion of substances first NaOH, 25% TEAOH (tetraethylammonium hydroxide) aqueous solution and NaAlO 2 Mix and stir until clear, then slowly add silica, and stir the resulting mixture for 1 h to obtain a transparent viscous gel. After the gel was completely dried in a vacuum oven at 70°C, it was ground and transferred to a 20 mL polytetrafluoroethylene liner, and then the liner containing the precursor was placed in another 100 mL liner with 0.5 mL deionized water at the bottom. The polytetrafluoroethylene lining was transferred to a hydrothermal reaction kettle for crystallization at 150°C for 24h. Wash the obtained solid with water and ethanol, dry it, and heat it up to 550°C at a rate of 1.67°C / min for 4 hours to remove the template agent, and then use 1.0mol / L NH 4 The Cl solution was ion-exchanged at 80° C. for 1 h, filtered, washed and dried, and then calcined in a muffle furnace at 55...

Embodiment 2

[0021] SiO 2 :Na 2 O: Al 2 o 3 :TEAOH:H 2 O = 1: 0.064: 0.04: 0.43: 10.5 The proportion of substances first NaOH, 25% TEAOH (tetraethylammonium hydroxide) aqueous solution and NaAlO 2 Mix and stir until clear, then slowly add silica, and stir the resulting mixture for 1 h to obtain a transparent viscous gel. After the gel was completely dried in a vacuum oven at 70°C, it was ground and transferred to a 20 mL polytetrafluoroethylene liner, and then the liner containing the precursor was placed in another 100 mL liner with 0.5 mL deionized water at the bottom. The polytetrafluoroethylene lining was transferred to a hydrothermal reaction kettle for crystallization at 150°C for 24h. Wash the obtained solid with water and ethanol, dry it, and heat it up to 550°C at a rate of 1.67°C / min for 4 hours to remove the template agent, and then use 1.0mol / L NH 4 The Cl solution was ion-exchanged at 80° C. for 1 h, filtered, washed and dried, and then calcined in a muffle furnace at 55...

Embodiment 3

[0026] SiO 2 :Na 2 O:Al 2 o 3 :TEAOH:H 2 O = 1: 0.064: 0.04: 0.43: 10.5 The proportion of substances first NaOH, 25% TEAOH (tetraethylammonium hydroxide) aqueous solution and NaAlO 2 Mix and stir until clear, then slowly add silica, and stir the resulting mixture for 1 h to obtain a transparent viscous gel. After the gel was completely dried in a vacuum oven at 70°C, it was ground and transferred to a 20 mL polytetrafluoroethylene liner, and then the liner containing the precursor was placed in another 100 mL liner with 0.5 mL deionized water at the bottom. The polytetrafluoroethylene lining was transferred to a hydrothermal reaction kettle for crystallization at 150°C for 24h. Wash the obtained solid with water and ethanol, dry it, and heat it up to 550°C at a rate of 1.67°C / min for 4 hours to remove the template agent, and then use 1.0mol / L NH 4 The Cl solution was ion-exchanged at 80° C. for 1 h, filtered, washed and dried, and then calcined in a muffle furnace at 550...

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Abstract

The invention discloses a method for catalyzing a dimerization-hydrogenation two-stage one-pot reaction of alpha-pinene in an intermittent autoclave reactor by adopting Ru metal nanoparticle coupled SOT-Hbeta zeolite as a bifunctional microporous molecular sieve catalyst. The method is characterized in that a seed crystal-organic template method is adopted to construct an Hbeta zeolite skeleton with proper acidity and shape selectivity so as to reduce the use of an organic template; the metal nanoparticles are introduced by adopting an isopyknic alcohol solution impregnation method and a hydrogen reduction method so as to ensure that the catalyst has high activity of both a metal component and a zeolite acid component. The one-pot reaction catalysis method is simple in process operation and excellent in reaction performance, the catalyst is easy to separate and reuse, and a clean and efficient new method is provided for preparation of the turpentine-based biomass high-energy-density fuel.

Description

technical field [0001] The invention relates to a method for catalyzing the dimerization-hydrogenation reaction of α-pinene, specifically a method for catalyzing the dimerization-hydrogenation reaction of α-pinene in one pot by using a bifunctional microporous molecular sieve catalyst. Background technique [0002] Among the abundant and cheap renewable natural resources, the efficient development and utilization of the unsaturated hydrocarbon α-pinene with a unique polycyclic structure has always been an important branch of biomass refining. α-pinene is the main component of turpentine, and its properties are relatively active. At present, it mainly prepares downstream products used in medicine, flavors and fragrances, printing and dyeing industries through isomerization, hydrogenation, hydration, oxidation, esterification and other reactions. In recent years, it has been found that α-pinene has a high-tension polycyclic structure composed of multiple closed ring planes, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/40C07C2/12C07C2/52C07C13/64B01J29/74B01J37/30B01J37/02C01B39/04
CPCC07C2/12C07C2/52B01J29/7415B01J37/30B01J37/0201B01J35/023C01B39/026C01B39/04B01J2229/186C07C2602/42C07C2603/52C07C13/40C07C13/64Y02P30/20
Inventor 袁冰朱本强解从霞于凤丽于世涛
Owner QINGDAO UNIV OF SCI & TECH
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