A method for preparing α-phenylethyl alcohol using zirconia-silica/graphene hybrid material as a catalyst

A technology of silica and hybrid materials, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the influence of zirconia grain dispersion uniformity, is not suitable for large-scale industrial applications, increases Catalyst energy consumption and other issues to achieve the effect of improving operational safety, reducing reaction energy consumption, and less impurities

Active Publication Date: 2016-08-24
湖州度信科技有限公司
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Problems solved by technology

For example, a method for preparing α-phenylethanol from an activated carbon alkaline earth metal oxide described in the published patent CN101792368A has high selectivity and short reaction time, but the alkaline earth metal has a negative effect on the moisture and CO in the air. 2 It is relatively sensitive, and it is easy to cause the deactivation of the active site of the catalyst and reduce the activity of the catalyst, and the catalyst needs to be calcined at high temperature
CN 101530792A discloses a supported zirconium oxide (ZrO 2 -Mg / Al-LDO) catalyst, used for the hydrogenation reduction of ketones to prepare the corresponding alcohol compounds, with high activity, this type of catalyst uses the magnesium-aluminum composite oxide Mg / Al-LDO obtained by roasting magnesium aluminum hydrotalcite as a carrier, The preparation process requires two high-temperature calcinations, which increases the energy consumption of the catalyst preparation process, and the dispersion uniformity of zirconia grains is seriously affected by the preparation conditions.
CN102190563A describes the method for preparing α-phenylethyl alcohol with MCM-41 supported zirconium oxide as a catalyst, and CN102211041A discloses a method for synthesizing α-phenylethyl alcohol with a mesoporous molecular sieve supported zirconia-third main group mixed oxide catalyst, And CN 102211045A describes that acetophenone prepares α-phenethyl alcohol through hydrogen transfer on the MCM-41 mesoporous molecular sieve supported zirconia-rare earth metal mixed oxide catalyst. The above three types of methods have mild reaction conditions, and the catalyst has high selectivity and high activity, but the preparation process of the catalyst carrier MCM-41 mesoporous molecular sieve uses a large amount of surfactant, which is expensive, and the carrier needs to be roasted at high temperature to remove the surfactant and emit a large amount of harmful gas, which pollutes the environment and the catalyst cost is high. The preparation conditions are complex and not suitable for large-scale industrial applications

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  • A method for preparing α-phenylethyl alcohol using zirconia-silica/graphene hybrid material as a catalyst
  • A method for preparing α-phenylethyl alcohol using zirconia-silica/graphene hybrid material as a catalyst
  • A method for preparing α-phenylethyl alcohol using zirconia-silica/graphene hybrid material as a catalyst

Examples

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Effect test

Embodiment 1-6

[0027] Example 1-6: Preparation of α-phenylethyl alcohol with different zirconia-silicon ratio zirconia-silicon dioxide / graphene hybrid materials as catalysts

[0028] 1. Preparation methods of zirconia-silicon dioxide / graphene hybrid materials with different zirconium-silicon ratios:

[0029] 1) Preparation of graphene oxide suspension: disperse graphene oxide in 10 ml of ethanol according to Table 1, and obtain a brown-yellow graphene oxide suspension after ultrasonication for 1-3 h;

[0030]2) Preparation of zirconia / silica-graphene wet gel: Mix 3.9 ml zirconyl nitrate, 10 ml ethanol and 15 ml acetic acid, and add to the graphene oxide suspension obtained in step 1), mix well and mark It is solution A; according to the different proportions in Table 1, take tetraethyl orthosilicate (TEOS), mix well with 1.5 ml of water, 1 ml of hydrochloric acid, and 10 ml of ethanol, and mark it as solution B. Add solution B dropwise to solution A, and let stand for 15 min to obtain zirco...

Embodiment 7-10

[0043] Example 7-10: The reaction results of preparing α-phenylethyl alcohol with different graphene doping amounts of zirconia-silicon dioxide / graphene hybrid materials as catalysts

[0044] Preparation of zirconia-silicon dioxide / graphene hybrid material with different graphene doping amounts: other conditions are as in Example 1, the difference is that step 1) is doped by different graphene in Table 2 Measure graphite oxide, step 2) Solution B is obtained by mixing 8 ml tetraethyl orthosilicate (TEOS), 1.5 ml water, 1 ml hydrochloric acid and 10 ml ethanol.

[0045] Catalytic reaction conditions: Other conditions are as the catalytic reaction conditions of embodiment 1-6, difference is that embodiment 7-10 adopts 0.2wt%, 0.5wt%, 1wt% and 2wt%ZrO successively 2 -SiO 2 / GO hybrid material as catalyst, the results are shown in Table 2.

Embodiment 11-17

[0053] Embodiment 11-17: the catalytic reaction result of different reaction time

[0054] Other conditions are as the catalytic reaction condition of embodiment 1-6, and difference is that embodiment 11-17 all adopts Zr:Si=1:2, 1wt%ZrO 2 -SiO 2 The / GO hybrid material was used as a catalyst, and different reaction times were used, ranging from 2 to 10 h. The results are shown in Table 3.

[0055] Table 3 Examples 11-17 catalytic reaction results

[0056]

[0057] As can be seen from Table 3, as the reaction time increases, the conversion of acetophenone of the present invention is first improved, and when the reaction exceeds 8 hours, the conversion rate of acetophenone decreases.

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Abstract

The invention discloses a method for preparing alpha-phenethyl alcohol by taking a zirconia-silica / graphene hybrid material as a catalyst and belongs to the technical field of chemical synthesis. The method comprises the following steps: by taking acetophenone as a raw material under normal pressure, taking alcohol as a hydrogen source and a solvent, and taking the zirconia-silica / graphene hybrid material as a catalyst, reacting at the reaction temperature of 45-90 DEG C for 2-10 hours, rectifying the reaction solution after the reaction is ended, taking the fraction at the temperature of 105-115 DEG C, thereby obtaining the alpha-phenethyl alcohol. According to the method disclosed by the invention, the zirconia-silica / graphene hybrid material is taken as the catalyst, the hybrid material is prepared by adding silica and doping graphene by virtue of an aerogel mode, the specific surface area and pore size of the catalyst are improved, dispersion of the surface active center is promoted, and the activity of the catalyst is increased. The catalyst is high in selectivity and high in water resistance, is easily separated in the reaction solution and can be repeatedly utilized after separation, the operation is convenient, and the preparation cost is reduced, so that the economic benefits are improved.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing α-phenylethyl alcohol by using a zirconia-silicon dioxide / graphene hybrid material as a catalyst. Background technique [0002] α-Phenylethyl alcohol is a compound widely used in aromatic compounds. It is mainly used in the synthesis of food flavors, various rose oils, essential oils and as an important pharmaceutical intermediate. At present, α-phenylethanol is mainly obtained from natural product extraction, microbial fermentation and organic synthesis. [0003] Extracted from natural essential oils, the source of raw materials for this method is limited, and the requirements for rectification equipment are high. [0004] As for the research on the production of natural-grade phenylethyl alcohol spices by microbial fermentation, related processes have been successfully developed at home and abroad in recent years. Huabao Aroma Tec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/22C07C29/143B01J21/18
CPCB01J21/18C07C29/143C07C33/22
Inventor 邓冰心张波姜剑锋
Owner 湖州度信科技有限公司
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