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Process for preparing beta-phenylethanol

A technology for phenethyl alcohol and chloroethyl alcohol, applied in the field of preparing β-phenethyl alcohol, can solve the problems of serious equipment corrosion, difficult to recover by-products, large consumption of benzene, etc. Effect

Inactive Publication Date: 2004-01-07
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the above-mentioned alkylation method for preparing β-phenylethanol, there are problems such as large consumption of benzene, serious equipment corrosion, difficulty in recycling by-products, and generation of a large amount of benzene-containing acidic wastewater to pollute the environment.

Method used

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  • Process for preparing beta-phenylethanol
  • Process for preparing beta-phenylethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] see figure 1 , the reaction equipment is mainly composed of ethylene oxide storage tank 1, jacketed alkylation reactor 2, jacketed hydrolyzer 3, concentration evaporator 4 and rectifier 5, and the reaction process is: alkylation Reaction → hydrolysis reaction → evaporation and concentration → rectification and purification, and further gel treatment.

[0027] (1) Alkylation

[0028] The alkylation reaction is carried out in an alkylation reactor. The alkylation reactor is a three-necked jacketed glass bottle with a stirring port, a ventilation port and a feeding port, with a volume of 250 milliliters, and 95% ethanol refrigeration circulation fluid is passed through the jacket as a cooling medium. The specific operation is: weigh 129 grams of benzene, put it into a constant weight alkylation reaction bottle, put a magnetic stirrer at the same time, start the circulating refrigerator and electromagnetic stirrer, and reduce the temperature of the reaction system to 5°C-...

Embodiment 2

[0037] (1) Alkylation

[0038] With embodiment 1. Calculate and pass into oxirane total amount 11.3 grams.

[0039] (2) Hydrolysis

[0040] Change the electromagnetic stirring of the above reactor into mechanical stirring, and install a feeding dropping funnel on the vent. Start the agitator, control the stirring speed to 500 rpm, and the hydrolysis temperature to 10-12°C, add 23 grams of deionized water to the reactor dropwise within 30 minutes, until the reaction system generates a transparent organic solution and a white wet gel solid. 140.2 grams of organic liquid in the upper layer was poured out, leaving 52.5 grams of gel in the reaction bottle.

[0041] (3) Evaporation and concentration

[0042] The organic liquid obtained by hydrolysis was transferred to a 250 mL distillation flask. After distillation, 114.6 grams of 99.9% benzene and 24.5 grams of β-phenylethanol concentrate were obtained.

[0043] (4) Distillation and refining

[0044]Pour 24.5 grams of β-phe...

Embodiment 3

[0048] Alkylation

[0049] With embodiment 1. Calculate and pass into oxirane total amount 11.6 grams.

[0050] (2) Hydrolysis

[0051] Change the electromagnetic stirring of the above reactor into mechanical stirring, and install a feeding dropping funnel on the vent. Start the agitator, control the stirring speed to be 500 rev / min, and the hydrolysis temperature is 5-6°C. In 30 minutes, add deionized water into the reactor four times, add 6 grams each time, add 24 grams of water in total, until The reaction system produces a transparent organic solution and a white wet gel solid. 140.3 grams of organic liquid in the upper layer was poured out, and 53.2 grams of gel remained in the reaction bottle.

[0052] (3) Evaporation and concentration

[0053] The organic liquid obtained after hydrolysis was transferred to a 250 mL distillation flask. After distillation, 113.8 grams of 99.9% benzene and 24.6 grams of β-phenylethanol concentrate were obtained.

[0054] (4) Distill...

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Abstract

The present invention discloses a method for preparing beta-phenylethanol from benzene and epoxyethane under the catalytic action of anhydrous alchlor, in the course of preparation it adopts the quantitative hydrolysis method so as to obtain the invented beta-phenylethanol.

Description

technical field [0001] The present invention relates to a method for preparing β-phenylethanol, in particular, it relates to a method for preparing high-purity β-phenylethanol and simultaneously recovering by-products chloroethanol and polyaluminum chloride, which are all useful chemical products . Background technique [0002] The English name of β-phenylethanol can be expressed as β-phenylethylalcohol or 2-benzeneethanol, molecular formula C 8 h 10 O, molecular weight 122.17. β-Phenylethyl alcohol is a colorless viscous liquid with a mild rose fragrance. β-Phenylethyl alcohol is mainly used in the manufacture of cosmetics and food fragrances and essences. [0003] In 1925, Schaarsschmidt A (Ber.1925, 58:1914) first proposed the method of directly synthesizing β-phenylethanol with benzene and ethylene oxide under the action of aluminum trichloride by Friedel-Crafts reaction. The more representative foreign patents in this respect are JP174230 (1949); US2483323 (1949) an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/10C07C33/22
Inventor 孙志强徐杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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