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Preparation method of 2, 3, 5-trimethyl benzoquinone (TMBQ)

A technology of trimethylbenzoquinone and triethylamine hydrochloride, applied in 2 fields, to achieve the effects of mild reaction conditions, promotion of catalytic oxidation, and high selectivity

Inactive Publication Date: 2012-08-15
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In summary, there are still big problems in the green process of efficient catalytic oxidation of TMP to prepare TMBQ, such as the development of low-cost and high-activity catalysts, and the greening of solvents, etc.

Method used

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  • Preparation method of 2, 3, 5-trimethyl benzoquinone (TMBQ)
  • Preparation method of 2, 3, 5-trimethyl benzoquinone (TMBQ)
  • Preparation method of 2, 3, 5-trimethyl benzoquinone (TMBQ)

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Embodiment 1

[0017] The preparation method of 2,3,5-trimethylbenzoquinone provided in this embodiment comprises the following steps:

[0018] (1) the triethylamine hydrochloride of 0.0015mol and the FeCl of 0.00015mol 3 Mix, stir at 35 °C for 1 h, then add 0.0030 mol of CuCl 2 , continue to stir for 1 hour at 35 ° C, and finally add 10 drops of concentrated HCl, continue to stir for 1 hour to prepare a composite catalyst;

[0019] (2) Dissolve 0.015mol of TMP in 25mL of acetic acid, mix well, and prepare a TMP acetic acid solution whose concentration is 0.6mol / L;

[0020] (3) Add the composite catalyst prepared in step (1) into the TMP acetic acid solution prepared in step (2), stir vigorously to make it evenly mixed, then heat to reflux under vigorous stirring to obtain reaction system A, and then start the peristaltic Pump, add hydrogen peroxide aqueous solution dropwise to reaction system A, the hydrogen peroxide aqueous solution contains 0.45mol of H 2 o 2 , the volume percentage c...

Embodiment 2

[0023] The preparation method of 2,3,5-trimethylbenzoquinone provided in this embodiment comprises the following steps:

[0024] (1) the triethylamine hydrochloride of 0.0015mol and the FeCl of 0.00015mol 3 Mix and stir at 35 °C for 1 h, then add 0.0015 mol of CuCl 2 , continue stirring at 35°C for 1 hour to obtain a composite catalyst;

[0025] (2) The TMP of 0.015mol and the benzoic acid of 0.0048mol are dissolved in 50mL ethanol, mix uniformly, make solution B, the concentration of TMP in solution B is 0.3mol / L;

[0026](3) Add the composite catalyst prepared in step (1) to the solution B prepared in step (2), stir vigorously to make it evenly mixed, then heat to reflux under vigorous stirring to obtain reaction system A, and then turn on the peristaltic pump , add dropwise hydrogen peroxide aqueous solution to the reaction system A, the hydrogen peroxide aqueous solution contains 0.45mol of H 2 o 2 , the volume percent concentration of the hydrogen peroxide aqueous sol...

Embodiment 3

[0029] The preparation method of 2,3,5-trimethylbenzoquinone provided in this embodiment comprises the following steps:

[0030] (1) the triethylamine hydrochloride of 0.0015mol and the FeCl of 0.00015mol 3 Mix and stir at 35 °C for 1 h, then add 0.0015 mol of CoCl 2 , continue stirring for 1 hour at 35°C to obtain a composite catalyst;

[0031] (2) 0.015mol of TMP was dissolved in 10mL of ethyl acetate, and mixed uniformly to obtain an ethyl acetate solution of TMP;

[0032] (3) Add the composite catalyst prepared in step (1) into the ethyl acetate solution of TMP prepared in step (2), stir vigorously to make it evenly mixed, then heat to reflux under vigorous stirring to obtain reaction system A, Afterwards, the peristaltic pump was turned on, and an aqueous hydrogen peroxide solution was added dropwise to the reaction system A, which contained 0.50mol of H 2 o 2 , the volume percent concentration of the hydrogen peroxide aqueous solution is 20%. After the hydrogen perox...

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Abstract

The invention discloses a preparation method of 2, 3, 5-trimethyl benzoquinone (TMBQ), which comprises the following steps of: (1) mixing CuCl2 and / or CoCl2, ferric chloride and triethylamine hydrochloride, evenly stirring and preparing a composite catalyst; (2) dissolving trimethylolpropane (TMP) in an organic solvent and preparing a TMP organic solvent solution; and (3) adding the prepared composite catalyst into the TMP organic solvent solution, stirring, evenly mixing, heating until backflow, dropwise adding a hydrogen peroxide aqueous solution and then carrying out reaction for 2-8hours at the temperature of 20-80 DEG C, and cooling the reaction solution to room temperature; and finally obtaining the TMBQ product after separating and purifying. The preparation method of the 2, 3, 5- TMBQ adopts TMP catalytic oxidation for one-step synthesis of TMBQ, and is a green technology, the oxidizing agent and solvent which are adopted by the preparation method have the advantages of being low in toxicity and harmless, the composite catalyst has high activity, and the transformation rates of the TMP and the selectivity of the TMBQ are high.

Description

technical field [0001] The invention relates to the technical field of vitamin E synthesis, in particular to a preparation method of 2,3,5-trimethylbenzoquinone. Background technique [0002] Vitamin E is an important fat-soluble biological antioxidant, which is widely used in medicine, health products, food, cosmetics, animal husbandry and other fields. The current market demand has exceeded 30,000 tons per year. 2,3,5-Trimethylhydroquinone (TMHQ) is an important intermediate in the synthesis of vitamin E and restricts the production of vitamin E. The production process of TMHQ includes the tricresyl method, the tricresyl method and the tricresyl method, in which 2,3,6-trimethylphenol (TMP) is directly oxidized to obtain 2,3,5-trimethylbenzoquinone (TMBQ ), and then the two-step process of obtaining TMHQ through reduction is the simplest. The raw material TMP of this process is rich in sources, the conversion rate of TMP and the selectivity of TMBQ are high, the process is...

Claims

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Application Information

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IPC IPC(8): C07C50/02C07C46/06B01J31/30
Inventor 毛立群杨俊娟刘勇李西营
Owner HENAN UNIVERSITY
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