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Preparation method of beta-phenylethyl alcohol

A technology for phenethyl alcohol and benzyl alcohol, which is applied in the field of preparing beta-phenethyl alcohol, can solve the problems of difficult recovery of catalyst, complex catalyst system, low catalyst selectivity, etc., and achieves low production cost, high activity and selectivity, and high selectivity high sex effect

Active Publication Date: 2017-08-25
SHANDONG NHU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The advantage of this method is that the reaction route is simple, and the disadvantage is that high pressure reaction is required, the requirements for equipment are high, the catalyst system is complex, the recovery and application of the catalyst is difficult, the selectivity of the catalyst is low, a large amount of toluene is produced by-product, the production cost is high, and industrial application is difficult. Big

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  • Preparation method of beta-phenylethyl alcohol
  • Preparation method of beta-phenylethyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 A kind of preparation method of β-phenylethyl alcohol

[0037] Include the following steps:

[0038] (1) Add catalyst, water, benzyl alcohol

[0039] Add 1g of ruthenium chloride, 6.8g of sodium triphenylphosphinetriisosulfonate TPPTS, and 300g of water into a 1000ml autoclave with magnetic stirring and a temperature controller; then add 200g of benzyl alcohol, replace it with nitrogen three times, and then use Replaced by hydrogen three times.

[0040] (2) Pass CO, H 2 mixed gas

[0041] Heating to 150°C, CO / H 2 The molar ratio of the mixed gas of 1:2 is pressurized to 6.0MPa, and the mixed gas,

[0042] Keep feeding to maintain the system pressure at 6.0MPa.

[0043] (3) Reaction

[0044] Stir at a speed of 700rpm, and take samples during the reaction to analyze the progress of the reaction. When the conversion rate of benzyl alcohol is greater than 60%, cool it with water, press out the reaction liquid, let it stand for stratification, and the wat...

Embodiment 2

[0046] Embodiment 2 A kind of preparation method of β-phenylethyl alcohol

[0047] Include the following steps:

[0048] (1) Add catalyst, water, benzyl alcohol

[0049] 1g rhodium chloride and 2.0g1,3,5-triaza-7-phosphoradamantane TPA, 300g water are joined in the 1000ml autoclave that has magnetic stirring and thermostat; Then add 200g benzyl alcohol, use Nitrogen was replaced three times, followed by hydrogen replacement three times.

[0050] (2) Pass CO, H 2 mixed gas

[0051] Heating to 150°C, CO / H 2 The mixed gas with a molar ratio of 1:1 is pressurized to 4.0MPa, and the mixed gas is continuously fed to maintain the system pressure at 4.0MPa.

[0052] (3) Reaction

[0053] Stir at 700rpm, take samples during the reaction and analyze that the conversion rate of benzyl alcohol is greater than 60%, cool it with water, press out the reaction solution, let it stand for stratification, the water phase containing the catalyst can continue to be applied to the next batch ...

Embodiment 3

[0055] Embodiment 3 A kind of preparation method of β-phenylethyl alcohol

[0056] Include the following steps:

[0057] (1) Add catalyst, water, benzyl alcohol

[0058] Add 1g of carbonyl rhodium acetylacetonate and 8.0g of 1.1'-binaphthyl-2.2'-sodium diphenylphosphine bisulfonate BINAPS, 300g of water into a 1000ml autoclave with magnetic stirring and a thermostat; then add 200g of benzene Methanol was replaced three times with nitrogen, and then three times with hydrogen.

[0059] (2) Pass CO, H 2 mixed gas

[0060] Heating to 100°C, CO / H 2 The mixed gas with a molar ratio of 1:2 is pressurized to 6.0MPa, and the mixed gas is continuously fed to maintain the pressure of the system at 6.0MPa.

[0061] (3) Reaction

[0062] Stir at 700rpm, sample and analyze the conversion rate of benzyl alcohol during the reaction process is greater than 60%, cool with water, press out the reaction solution, let it stand for stratification, the water phase containing the catalyst can con...

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Abstract

The invention provides a preparation method of beta-phenylethyl alcohol. The preparation method comprises the following steps: adding a catalyst, water and benzyl alcohol, introducing mixed gas of CO and H2, and reacting. The catalyst has high activity and selectivity, conversion ratio of the benzyl alcohol is more than 50%, and the total selectivity of beta-phenylethyl alcohol and phenylacetaldehyde is more than 90%. The preparation method provided by the invention has the advantages that a water soluble complex catalyst formed by water soluble ruthenium and rhodium metal salts and a water soluble ligand is used for carrying out homologation on the benzyl alcohol in a water-oil two-phase system, and better activity and selectivity can be obtained compared with the traditional cobalt-ruthenium homogeneous catalysis system; water and oil phases react, aftertreatment is convenient, a water-phase catalyst can be recycled, environment friendliness is realized, and fewer three wastes are discharged.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing beta-phenylethanol from benzyl alcohol. Background technique [0002] β-phenylethanol (2-phenylethanol) is an aromatic alcohol with a soft and delicate rose smell, which is widely used in rose-type and other types of fragrance formulas, and is widely used in the fields of medicine, food and daily chemicals. The consumption of β-phenylethanol in the world is about 20,000 tons / year. [0003] The methods for synthesizing β-phenylethanol in the prior art mainly include haloalcohol method, benzene-ethylene oxide alkylation method and styrene oxide hydrogenation method. Wherein the phenylethanol prepared by the benzene-ethylene oxide alkylation method has more impurities and is difficult to use as a perfume. Haloalcohol method and styrene oxide hydrogenation method are common methods for producing β-phenylethanol in industry. At present, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/32C07C29/141C07C33/22C07C45/50C07C47/228B01J31/24
CPCB01J31/2409B01J2531/822C07C29/141C07C29/32C07C45/50C07C33/22C07C47/228Y02P20/584
Inventor 赵文乐马啸马书召李文涛郝小雷王军吕爱凝
Owner SHANDONG NHU PHARMA
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