Synthesis method of alpha phenyl ethanol

A synthesis method and technology of phenylethyl alcohol, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of easy environmental pollution, low synthesis selectivity, complicated operation, etc., and achieve high utilization rate , high product selectivity and simple process

Inactive Publication Date: 2007-02-14
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the shortcomings in the prior art that the synthesis selectivity of α-phenylethanol is not high, it is easy to cause pollution to the environment, the cost is high, and the operation is complicated, the present invention provides a product with high selectivity, no pollution to the environment, and low production cost. , a method for synthesizing α-phenylethanol in one step by in-situ hydrogenation of acetophenone with simple process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 2.5g of Raney nickel catalyst (3.4mL bulk volume) in the fixed-bed reactor, the ratio of the amount of acetophenone, methanol, water substance is 1: 15: 20 mixed liquid with the liquid hourly space velocity being 0.706 hours -1Add it into the reactor, adjust the reaction temperature to 120°C, and the reaction pressure to 0.4MPa. The product at the outlet of the reactor is separated from the liquid product by a gas-liquid separator. The conversion rate of ethyl ketone is 36.59%, the selectivity of α-phenylethanol is 83.81%, and the selectivity of by-product ethylbenzene is 16.19%.

Embodiment 2

[0024] Add 2.5g of Raney nickel catalyst (3.4mL bulk volume) in the fixed-bed reactor, the ratio of the amount of acetophenone, methanol, water substance is 1: 15: 20 mixed liquid with the liquid hourly space velocity being 0.706 hours -1 Add it into the reactor, adjust the reaction temperature to 130°C, and the reaction pressure to 0.52MPa. The product at the outlet of the reactor is separated from the liquid product by a gas-liquid separator, and the liquid product is analyzed by Agilent-GC-MS. The conversion rate of ethyl ketone was 40.41%, the selectivity of α-phenylethanol was 90.35%, and the selectivity of by-product ethylbenzene and α-cyclohexyl alcohol were 9.09% and 0.56%, respectively.

Embodiment 3

[0026] Add 2.5g of Raney nickel catalyst (3.4mL bulk volume) in the fixed-bed reactor, the ratio of the amount of acetophenone, methanol, water substance is 1: 15: 20 mixed liquid with the liquid hourly space velocity being 0.706 hours -1 Add it into the reactor, adjust the reaction temperature to 140 ° C, and the reaction pressure to 0.7 MPa. The product at the outlet of the reactor is separated from the liquid product by a gas-liquid separator. The conversion rate of ethyl ketone is 47.59%, the selectivity of α-phenylethanol is 77.35%, and the selectivity of by-product ethylbenzene, α-cyclohexyl ethanol, cyclohexyl ethyl ketone and cyclohexyl ethane are 22.06%, 0.29% respectively , 0.20% and 0.11%.

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Abstract

The present invention relates to alpha-phenyl ethyl alcohol synthesizing process, and is especially one in-situ acetophenone hydrogenating process of synthesizing alpha-phenyl ethyl alcohol. Inside the mixed solution of C1-C4 fatty alcohol and water and under the action of Raney nickel catalyst, acetophenone is one-step reacted at 50-300 deg.c and 0.1-10.0 MPa to obtain alpha-phenyl ethyl alcohol. The weight ratio of acetophenone, C1-C4 fatty alcohol and water is 1 to 2.5-60 to 10-160. The present invention has the beneficial effects of no need of outer hydrogen supply, simple technological process, low production cost, use of non-noble metal Raney nickel catalyst, high acetophenone converting rate, high alpha-phenyl ethyl alcohol selectivity up to 90 %, less side products and capacity of separating high purity alpha-phenyl ethyl alcohol.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing alpha-phenylethanol, in particular to a method for synthesizing alpha-phenylethanol by in-situ hydrogenation of acetophenone. (2) Background technology [0002] α-Phenylethyl alcohol is an important chemical product, which is widely used in pharmaceutical industry and fragrance manufacturing industry. In the fragrance manufacturing industry, α-phenylethanol is widely used for aroma reconciliation, and as the main component of rose fragrance, it is used in the synthesis of various rose oils and essential oils. α-Phenethyl alcohol is an important drug intermediate in the synthesis of many drugs, such as ibuprofen, an important raw material for the synthesis of non-steroidal sedative drugs. The existing α-phenylethanol synthesis methods include: organic synthesis and microbial fermentation. [0003] The organic synthesis method uses acetophenone as the starting material to react to obtain α-phenylet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/22C07C29/145B01J25/02
Inventor 李小年姜莉
Owner ZHEJIANG UNIV OF TECH
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