A kind of method for preparing dihydrocitronellal

A technology of dihydrocitroninum and malal, which is applied to the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of increasing post-processing steps and costs, and achieve easy control, simple methods, and Avoid the effects of high temperature and pressure conditions

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Both S.H.Liu and Zhang Yahong used metal alkoxide single salts in their experiments. The positive effect lies in the selective hydrogenation of carbon-oxygen double bonds, but no reduction effect on carbon-carbon double bonds. The solvent involved in the reaction increases the steps and costs of post-processing;

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  • A kind of method for preparing dihydrocitronellal

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preparation example Construction

[0046] The preparation method of iron cobalt n-decoxide

[0047] (1) ferric chloride and n-decyl alcohol that the mol ratio is 1:3 are put into the round-bottomed flask, the flask is placed in an oil bath and heated, reacted at 250 ° C for 8 hours, and distillation under reduced pressure obtains iron n-decyl alcohol;

[0048] (2) the cobalt chloride and n-decanol that the mol ratio is 1:3 are put into the round-bottomed flask, the flask is placed in an oil bath and heated, and reacted at 250 ° C for 8 hours, and distillation under reduced pressure obtains cobalt n-decoxide;

[0049] (3) Ferric n-decoxide and cobalt n-decoxide with a molar ratio of 1:1 are put into a round-bottomed flask, and benzene is used as a solvent, and the reaction time is 12 hours at 280° C., and distillation under reduced pressure is performed to obtain iron cobalt n-decoxide.

[0050] exist figure 1 In the infrared spectrum of 576cm -1 , 540.38cm -1 , 468.84cm -1 , is the absorption peak of iron c...

Embodiment 1

[0054] A method for preparing dihydrocitronellal, the steps are:

[0055] Under the protection of nitrogen atmosphere, 0.152g iron cobalt n-decoxide, 3.04g (5% nickel loading) nickel activated carbon, 64g methanol and 152.1g citral (acid value 0.05mgKOH / g) were added to the reaction kettle. After 6 times of replacement with nitrogen and the volume content of oxygen reduced to below 10 ppm, heating was started, the temperature of the reaction kettle was raised to 30 °C, the pressure was normal pressure, and the reaction was maintained at the temperature of the kettle for 20 h. After the reaction was completed, the reaction solution was obtained by filtration.

[0056] A small amount of the reaction solution was analyzed by gas chromatography, and the conversion rate of citral was 99.01%, and the selectivity of the main product, dihydrocitronellal, was 98.39%. The conversion rate of methanol is 99.5%, and the selectivity of converting methanol into target by-product formaldehyd...

Embodiment 2

[0059] A method for preparing dihydrocitronellal, the steps are:

[0060] Under the protection of nitrogen atmosphere, 0.304g iron cobalt n-decoxide, 30.42g (5% nickel loading) nickel carbon nanotubes, 110.4g ethanol and 152.1g citral (acid value 0.05mgKOH / g) were added to the reaction kettle. After 6 times of nitrogen replacement, the oxygen volume content dropped below 10 ppm, and then the heating was started, the temperature of the reaction kettle was raised to 40 °C, the pressure was normal pressure, and the reaction was maintained at the kettle temperature for 6 h. After the reaction was completed, the reaction solution was obtained by filtration.

[0061] A small amount of the reaction solution was analyzed by gas chromatography. The conversion rate of citral was 99.24%, and the selectivity of the main product, dihydrocitronellal, was 98.61%. The conversion rate of ethanol is 83.71%, and the selectivity of converting ethanol into the target by-product formaldehyde is 98...

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Abstract

The present invention provides a method for preparing dihydrocitronellal. Using raw material citral as hydrogen acceptor and alcohol compound as hydrogen donor, intermolecular hydrogen transfer reaction takes place under the action of catalyst system to obtain dihydrocitronellal; the citral acid value is required to be less than 0.1mgKOH/g ; The catalyst system includes: a heterogeneous nickel-based catalyst component includes nickel, a carrier, and a bimetallic alkoxide. The reaction pressure of the invention is normal pressure, the reaction temperature is low, the control is easy, the catalyst is cheap and easy to obtain, the product selectivity and the raw material conversion rate are high, and the by-product selectivity is high, and the dihydrocitronellal can be easily separated by means of rectification. , the method is simple and easy to implement, suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a method for preparing dihydrocitronellal, in particular to a method for preparing dihydrocitronellal from citral. Background technique [0002] Dihydrocitronellal is a terpenoid compound and an intermediate in organic synthesis. It can be used as a fungicide in the food industry itself. Since the structure of insect juvenile hormone was determined, its application value has been further improved. [0003] Jyri et al. (Silca supported ionic liquid catalysts for fine chemical[J].Appl CatalA:General,2007,328:68-76.) used ionic liquids and Pd ions to dissolve in acetone and loaded on activated carbon cloth to ensure the citral When the conversion rate is 100%, the selectivity of dihydrocitronellal can reach 88%; Pascal et al. (Pressure dependent product distribution of citral hydrogenation over micellehosted Pd and Ru nanoparticles in supercritical carbon dioxide [J]. J Cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/62C07C47/02
CPCC07C45/62C07C47/02Y02P20/54
Inventor 于斌成王联防董菁张永振
Owner WANHUA CHEM GRP CO LTD
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