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A kind of preparation method of 3-buten-1-ol

A technology of butene and allyl bromide, applied in the field of preparation of 3-butene-1-ol, can solve the problems of complicated production operation, high reaction temperature, long reaction time, etc. Simple, easy-to-use effects

Active Publication Date: 2022-05-17
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are some deficiencies in the preparation methods of some currently disclosed 3-buten-1-ols: in the method disclosed in CN102320926, the solvent tetrahydrofuran used in the reaction is miscible with water, and recovery is difficult. Dichloromethane is used as the extraction agent, which is a non-environmental solvent. Using a catalyst, the reaction time is long, the water phase needs to be extracted multiple times, the reaction liquid needs to be pretreated, and the production operation is complicated
The disclosed method of CN10759529, its reaction temperature is too high, operation difficulty is big, is unfavorable for industrialized production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Add 350 liters of ethyl acetate, 100 liters of allyl bromide, 120 kg of zinc powder, 150 liters of formaldehyde, and 3 kg of copper salt into the reactor. The reaction is exothermic, and the temperature is controlled below 75 ° C. Stir the reaction for 5 hours , 90 kilograms of ammonium chloride was added to the reactor, and the reaction was stirred for 2 hours;

[0016] (2) Stop stirring, let it stand for 1 hour, and separate the organic phase and the water phase;

[0017] (3) The separated aqueous phase is decompressed at 50-80°C and the vacuum degree is 0.055-0.075Mp to distill the organic components;

[0018] (4) The organic phase obtained in (2) was mixed with the organic component obtained in (3), ethyl acetate was distilled off under normal pressure, and 74 kg of 3-buten-1-ol was distilled off under reduced pressure at 80°C. Yield 87%, purity 99.2%.

Embodiment 2

[0020] (1) Add 300 liters of ethyl acetate, 100 liters of allyl bromide, 100 kg of zinc powder, 130 liters of formaldehyde, and 2 kg of copper salt into the reactor. The reaction is exothermic, and the temperature is controlled below 75 ° C. Stir the reaction for 4 hours , 70 kg of ammonium chloride was added to the reactor, and the reaction was stirred for 1.5 hours;

[0021] (2) Stop stirring, let it stand for 1 hour, and separate the organic phase and the water phase;

[0022] (3) The separated aqueous phase is decompressed at 50-80°C and the vacuum degree is 0.055-0.075Mp to distill the organic components;

[0023] (4) The organic phase obtained in (2) was mixed with the organic component obtained in (3), ethyl acetate was distilled off under normal pressure, and 72 kg of 3-buten-1-ol was distilled off under reduced pressure at 80°C. Yield 85%, purity 99.2%.

Embodiment 3

[0025] (1) Add 250 liters of ethyl acetate, 100 liters of allyl bromide, 80 kg of zinc powder, 110 liters of formaldehyde, and 1 kg of copper salt into the reactor. The reaction is exothermic, and the temperature is controlled below 75 ° C. Stir the reaction for 3 hours , 50 kg of ammonium chloride was added to the reaction kettle, and the reaction was stirred for 1 hour;

[0026] (2) Stop stirring, stand still for 0.5h, and separate the organic phase and the water phase;

[0027] (3) The separated aqueous phase is decompressed at 50-80°C and the vacuum degree is 0.055-0.075Mp to distill the organic components;

[0028] (4) The organic phase obtained in (2) was mixed with the organic component obtained in (3), ethyl acetate was distilled off under normal pressure, and 62 kg of 3-buten-1-ol was distilled off under reduced pressure at 80°C. Yield 74%, purity 99.2%.

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Abstract

The invention relates to a preparation method of 3-butene-1-alcohol, using ethyl acetate as solvent, raw materials are allyl bromide, zinc powder, formaldehyde, ammonium chloride, catalyst is copper salt, and the reaction product is 3 ‑Butene‑1‑alcohol. The reaction yield is greater than 87%, and the purity is greater than 99%. In order to make up for the deficiencies of the existing disclosed technology, the present invention greatly reduces the reaction time by adding a catalyst; the distillation method is used instead of multiple extractions to treat the reaction water phase, the operation is more convenient and the cost is greatly reduced; the environment-friendly organic matter is used as a solvent, which is in line with environmental protection production concept.

Description

technical field [0001] The invention relates to a preparation method of 3-buten-1-ol. Background technique [0002] 3-Butene-1-ol (BTO) is a kind of enol compound with very high added value. Because it has double bonds and hydroxyl groups in its molecule, it is very active in nature, high in reactivity, and prone to esterification, Addition, oxidation and reduction and other chemical reactions are widely used in many fields such as petrochemical industry, food flavor, agrochemical products, pharmaceutical synthesis, etc. ) important pharmaceutical intermediates. In recent years, with the sharp increase in the incidence of tumor diseases, the market demand for 3-buten-1-ol has greatly increased. In view of the current situation, it is urgent to develop a better synthetic method with easy-to-obtain raw materials, simple process, green environmental protection and low cost. There are some deficiencies in the preparation methods of some currently disclosed 3-buten-1-ols: in t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/40C07C29/86C07C29/80C07C33/025C07F3/06
CPCC07C29/40C07C29/86C07C29/80C07F3/06C07C33/025Y02P20/584
Inventor 孙国新赵建国赵奕铭
Owner UNIV OF JINAN
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