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Method for continuously producing vinyl-beta-ionol

A technology of ionol and vinyl, applied in chemical instruments and methods, preparation of organic compounds, magnesium chloride, etc., can solve problems such as unmentioned vinyl-β-ionol production process, difficult production process, complicated post-treatment, etc. , to achieve the effect of being suitable for large-scale industrial production, reducing reaction risk, and simple post-processing

Pending Publication Date: 2018-05-08
WANHUA CHEM GRP CO LTD
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Problems solved by technology

[0003] The document ""Synthesis of Vinyl-β-ionol", Shanghai Institute of Applied Technology" introduces its preparation method, which is a batch process, and does not mention the specific production process of vinyl-β-ionol. This method uses Saturated ammonium chloride is used as the quenching agent, the post-treatment is complicated, and the separation of its products produces a large amount of waste water, and the cost is high
The paper "Research on the New Process of Synthesizing Vitamin A by Wittig Method" introduced the acetylene hydrogenation of β-ionone, using acetylene, liquid ammonia, etc., which put forward high requirements for equipment, and at the same time brought great difficulties to the production process
[0004] There is no report on the production of vinyl-β-ionol by continuous Grignard reaction

Method used

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  • Method for continuously producing vinyl-beta-ionol

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Effect test

Embodiment 1

[0051] The tetrahydrofuran solution (molar concentration is 2mol / L, mass fraction is 16.39%) of vinyl chloride magnesium and β-ionone enters in the static mixer with the feed rate of 991.43g / min, 200g / min respectively, and reaction temperature is 5 °C, the residence time is 200s, and the intermediate is obtained from the reaction. After the reaction finishes, the intermediate enters the quenching reactor 2a, and when the reaction solution quality in the reactor 2a is 416kg, it stops feeding to the reactor 2a, and the intermediate enters the quenching reactor 2b, and the reactor 2a begins to feed at 140g / min Add 40kg of water at a high speed to quench, and the quenching temperature is 5°C. After the quenching is completed, move the product to a centrifugal filter and filter it with a 1500-mesh filter cloth, separate the filtrate at a speed of 600rmp, and centrifuge to obtain basic magnesium chloride and filtrate ethylene. The tetrahydrofuran solution of β-ionol, the filter cake...

Embodiment 2

[0053]The tetrahydrofuran solution of magnesium vinyl chloride (molar concentration is 1mol / L, mass fraction is 8.9%) and β-ionone are entered in the static mixer with the feed rate of 1520g / min, 200g / min respectively, and the reaction temperature is 5 ℃ , the residence time is 500s, and the intermediate is obtained from the reaction. After the reaction finishes, the intermediate enters the quenching reactor 2a, and when the reaction liquid quality in the still is 601kg, stop feeding to the reactor 2a, the intermediate enters the quenching reactor 2b, and the reactor 2a begins to add 59kg at 200g / min Quenching with water, the quenching temperature is -2°C, after the quenching is completed, move the product to a centrifugal filter and filter it with a 3000-mesh filter cloth, separate the filtrate at a speed of 1000rmp, and centrifuge to obtain basic magnesium chloride and filtrate vinyl-β -The tetrahydrofuran solution of ionol, filter cake basic magnesium chloride adds 29kg tet...

Embodiment 3

[0055] The tetrahydrofuran solution (molar concentration is 1.5mol / L, 12.8%) of vinyl chloride magnesium and β-ionone enter in the static mixer with the feed rate of 775g / min, 200g / min respectively, and reaction temperature is 1 ℃, stops The time is 600s, and the intermediate is obtained from the reaction. After the reaction finishes, the intermediate enters the quenching reactor 2a. When the reaction liquid quality in the still is 426kg, it stops feeding to the reactor 2a, the intermediate enters the quenching reactor 2b, and the reactor 2a begins to add 72kg at 400g / min. Water is used for quenching, and the quenching temperature is -5°C. After quenching, the product is transferred to a centrifugal filter and filtered with a 2000-mesh filter cloth. The filtrate is separated at a speed of 600rmp, and centrifuged to obtain basic magnesium chloride and filtrate vinyl-β -The tetrahydrofuran solution of ionol, the basic magnesium chloride of filter cake adds 19.1kg tetrahydrofuran...

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Abstract

The invention provides a method for continuously producing vinyl-beta-ionol, which comprises the following steps: taking beta-ionone as a raw material, enabling the beta-ionone and a vinyl-magnesium chloride solution to enter a static mixer, and reacting to generate an intermediate; reacting the intermediate and water in a quenching reactor to generate vinyl-beat-ionol and basic magnesium chloride; centrifugally filtering to obtain a vinyl-beta-ionol solution, rectifying the vinyl-beta-ionol solution to obtain vinyl-beta-ionol. The method provided by the invention has the advantages that: (1)continuous production of vinyl-beta-ionol is realized; (2) safety in a Grignard reaction and a quenching process is improved; (3) the production technology flow is simplified, the production period isshortened, and the production cost is reduced.

Description

technical field [0001] The invention relates to a method for continuous production of vinyl-β-ionol, specifically using β-ionone and vinyl magnesium chloride as raw materials to continuously prepare vinyl-β-ionol through Grignard reaction. Background technique [0002] Vinyl-β-ionol is a key intermediate in the synthesis process of vitamin A and isotretinoin. Currently, the production methods of vinyl-β-ionol include acetylenic hydrogenation method and Grignard reaction method. [0003] The document ""Synthesis of Vinyl-β-ionol", Shanghai Institute of Applied Technology" introduces its preparation method, which is a batch process, and does not mention the specific production process of vinyl-β-ionol. This method uses Saturated ammonium chloride is used as the quenching agent, the post-treatment is complicated, and the separation of its products produces a large amount of waste water, which is costly. The paper "Study on New Technology of Synthesizing Vitamin A by Wittig Met...

Claims

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Application Information

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IPC IPC(8): C07C29/34C07C33/14C01F5/30
CPCC07C29/34C07C33/14
Inventor 王延斌吕英东张涛林龙
Owner WANHUA CHEM GRP CO LTD
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