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Preparation method of 4-vinyl guaiacol, and 4-vinyl guaiacol

A guaiacol and vinyl technology, which is applied in the field of preparation of 4-vinyl guaiacol, can solve the problems of poor catalyst catalytic effect, inability to continuously produce, poor product quality, etc., and achieves good product quality and reaction time. Short, productive results

Active Publication Date: 2018-10-12
TONGREN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Most of the 4-vinylguaiacol currently on the market is chemically synthesized, but the existing chemical synthesis process mainly has the following disadvantages: (1) most of them are batch reactions, which cannot be produced continuously, and the operation is complicated and the yield is low. Lower, the product quality that obtains is poor; (2) reaction time is long, and reaction speed is slow, generally needs 4-8 hour; (3) the product 4-vinyl guaiacol that reaction obtains is easy to polymerize into dimer (4) The catalytic effect of the catalyst used is poor, it is inconvenient to use, the service life is short, and the reaction cycle is long

Method used

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preparation example Construction

[0027] In a first aspect, a method for preparing 4-vinylguaiacol is provided in at least one embodiment, comprising the following steps:

[0028] Loading a solid superacid catalyst into a fixed-bed reactor, and then heating the fixed-bed reactor;

[0029] Input the mixture of ferulic acid and weakly basic organic solvent in fixed-bed reactor;

[0030] The mixture is decarboxylated under the action of a solid superacid catalyst to obtain a crude product of 4-vinylguaiacol, and the crude product is refined to obtain high-purity 4-vinylguaiacol.

[0031] The present invention is mainly aimed at the existing fluidized bed or reactor batch preparation process of 4-vinylguaiacol. The existing reaction temperature is low, the reaction speed is slow, and the reaction time is long, generally 4-8 hours. The product obtained by the reaction 4-Vinyl guaiacol is easy to polymerize into dimers, the yield is low, and the operation is cumbersome. A new method for the preparation of 4-vinyl g...

Embodiment 1

[0064] A preparation method for 4-vinyl guaiacol, comprising the following steps:

[0065] (a) In an adiabatic fixed-bed reactor with a diameter of 3.5 cm and a height of 80 cm, particle-type SO with a diameter of Φ = 4 to 6 mm 4 2- / M x o y 200g of solid superacid catalyst; the SO 4 2- / M x o y M in solid-like superacid catalysts x o y ZrO 2 、TiO 2 , SnO 2 Oxides or their composite oxides;

[0066] (b) dissolving ferulic acid with a mass ratio of ferulic acid and a weakly basic organic solvent of 1:2 to obtain a mixture; wherein the weakly basic organic solvent is pyridine;

[0067] (c) heating the fixed bed reactor to 150°C;

[0068] (d) input the mixture of ferulic acid and weakly basic organic solvent in fixed-bed reactor with mass space velocity 1.5g / min by pump;

[0069] (d) The mixture is decarboxylated under the action of a solid superacid catalyst to obtain a crude product containing 4-vinylguaiacol, and the crude product is decompressed to remove the so...

Embodiment 2

[0072] A kind of preparation method of 4-vinyl guaiacol, the difference with embodiment 1 is:

[0073] In step (b), the weakly basic organic solvent is N,N-dimethylacetamide, and the mass ratio of ferulic acid and weakly basic organic solvent is 1:3;

[0074] In step (c), the temperature is 150°C;

[0075] In step (d), the mass space velocity is 1.8g / min.

[0076] Through gas chromatography analysis, the GC purity of the product is 99.4%; after calculation, the molar yield of the product is 93%.

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Abstract

The invention belongs to the technical field of 4-vinyl guaiacol preparation, and relates to a preparation method of 4-vinyl guaiacol, and the 4-vinyl guaiacol. The preparation method comprises the following steps: filling a fixed bed reactor with a solid super acidic catalyst, and heating the fixed bed reactor; introducing a mixture of ferulic acid and a weakly alkaline organic solvent into the fixed bed reactor; performing a decarboxylic reaction on the mixture under the effect of the solid super acidic catalyst to obtain a crude product of 4-vinyl guaiacol; refining the crude product to obtain high-purity 4-vinyl guaiacol. The method is likely to realize continuous production and simple in process, so that the reaction yield is improved, generation of a polymer is greatly reduced, and the product quality is improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of 4-vinyl guaiacol, and in particular relates to a preparation method of 4-vinyl guaiacol and 4-vinyl guaiacol. Background technique [0002] 4-vinylguaiacol (4-Vinylguaiacol 4VG for short), scientific name 2-methoxy-4-vinylphenol (2-Methoxy-4-vinylphenol). Its molecular formula is C 9 h 10 o 2 , density 1.11×10 3 kg / m 3 , melting point 26°C-29°C, boiling point 100°C / 667Pa. It is a colorless or light yellow oily liquid under normal temperature and pressure, showing a fermented aroma, slightly sweet, slightly phenolic smell. Natural 4-vinylguaiacol mainly exists in the volatile matter of corn alcoholic fermentation, and has an aroma similar to cloves. It is the main aroma component that determines the quality of wine, soy sauce, tea, coffee, cheese and other foods. It is one of the more commonly used high-end spices in industries such as medicine, flavor synthesis, etc. Its commercial v...

Claims

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Application Information

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IPC IPC(8): C07C41/18C07C43/23
CPCC07C41/18C07C43/23
Inventor 李修刚叶小青丁谦吴宜佩李选维
Owner TONGREN UNIV
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