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The preparation method of α-phenethyl alcohol

A technology of phenylethyl alcohol and acetophenone, which is applied in the field of preparation of α-phenylethyl alcohol, can solve the problems of high cost, low synthesis selectivity, easy environmental pollution, etc., achieve short reaction time, mild reaction conditions, and reduce industrial production cost effect

Active Publication Date: 2019-12-31
ZHEJIANG PHARMA COLLEGE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the defects of low synthesis selectivity, easy pollution to the environment and high cost of α-phenylethanol in the prior art, the present invention provides a one-step synthesis method with high product selectivity, high conversion rate of raw materials and no pollution to the environment α-Phenethyl alcohol method

Method used

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Experimental program
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Embodiment 1

[0025] After adding 0.8g of 16.7% Co / mordenite catalyst, 5ml of acetophenone, and 160ml of solvent water into a 250ml stainless steel reactor, seal it, replace it with nitrogen and hydrogen for three times, feed hydrogen, and control the reaction pressure to 2MPa. It is 800r / min, and the reaction temperature is 100°C. After 6 hours of reaction, the product at the outlet of the reactor is separated from the liquid product through a gas-liquid separator, and the liquid product is analyzed by a gas chromatography spectrometer. , the selectivity of α-phenylethanol is 100%.

[0026] Except having changed the reaction conditions as shown in Table 1, it reacted and measured in the same manner as Example 1. Reaction condition and result are as shown in embodiment 2-4 in table 1:

[0027] Table 1 Hydrogenation of acetophenone on Co / mordenite catalysts to produce phenylethyl alcohol in different solvents

[0028]

[0029]

[0030] As can be seen from Table 1, when water is used ...

Embodiment 8 to Embodiment 11

[0036] Embodiment 8 to embodiment 11 investigate the impact of reaction time on conversion rate and selectivity

[0037] Except having changed the reaction conditions as shown in Table 3, it reacted and measured in the same manner as Example 1. Reaction condition and result are as shown in embodiment 8-11 in table 3:

[0038] Table 3 The influence of different reaction times in solvent water on the reaction of acetophenone hydrogenation to phenylethanol

[0039] time / h Acetophenone conversion rate (%) α-Phenethyl alcohol selectivity (%) Example 1 6 99.9 100 Example 8 2 52.3 100 Example 9 4 85.0 100 Example 10 8 100 99.8 Example 11 10 100 99.3

[0040] It can be seen from Table 3 that as the reaction time prolongs, the conversion rate of acetophenone increases, and the reaction time is preferably 6 to 10 hours.

[0041] Embodiment 12 to embodiment 16 investigates the influence of reaction temperature on conversion ra...

Embodiment 17

[0048] After adding 0.8g of 16.7% Co / Hβ catalyst, 5ml of acetophenone, and 160ml of solvent water in a 250ml stainless steel reactor, seal it, replace it with nitrogen and hydrogen for three times, feed hydrogen, control the reaction pressure to 2MPa, and the rotating speed is 800r / min, reaction temperature 100 DEG C, after reacting for 6 hours, the product of reactor outlet is separated liquid product through gas-liquid separator, and liquid product is analyzed with mass spectrometry instrument, and the transformation rate of acetophenone is 97.1%, The selectivity of α-phenylethanol is 97.5%.

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Abstract

The invention provides a preparation method for alpha-phenethanol. The preparation method for alpha-phenethanol comprises the following steps: adding a raw material acetophenone, a solvent water and a catalyst into a reactor, wherein the catalyst is a supported cobalt-based catalyst or a supported copper-based catalyst; sealing the reactor, and replacing with nitrogen gas and hydrogen gas for three times respectively; and providing a hydrogen gas source, controlling the pressure in the reactor to be 0.50-3 MPa and the stirring speed to be 500-1000 rpm, carrying out a reaction for 2-10 hours at the temperature of 70-120 DEG C, and carrying out a one-step reaction to obtain the alpha-phenethanol. The alpha-phenethanol prepared by the process has the advantages of high conversion rate and high selectivity and is pollution-free to the environment with water as the solvent, and the industrial feasibility is greatly improved.

Description

【Technical field】 [0001] The invention relates to a preparation method of α-phenylethanol, in particular to a method for synthesizing α-phenylethanol by in-situ hydrogenation of acetophenone. 【Background technique】 [0002] α-Phenyl alcohol is widely used in the pharmaceutical and perfume industries. At present, aluminum isopropoxide or lithium aluminum hydride is usually used in industry to reduce α, β-unsaturated aldehydes (ketones) to prepare α, β-unsaturated alcohols. Although the method of reducing inorganic substances can obtain high-yield α, β-unsaturated alcohols, the remaining metal ions are discharged as waste liquid, which not only increases the difficulty of separating the product from the system, but also pollutes the environment. The heterogeneous catalytic hydrogenation technology uses hydrogen as the reducing agent, with 100% atom economy, and has the advantages of easy catalyst preparation, easy separation from the reaction system after the reaction, and reu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/145C07C33/22
CPCC07C29/145C07C33/22
Inventor 张新波张斌张雅娟秦永华许莉勇戴静波
Owner ZHEJIANG PHARMA COLLEGE
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