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Preparation method of trimethyl hydroquinone

A technology of trimethylhydroquinone and trimethylbenzoquinone, which is applied in the field of preparation of trimethylhydroquinone, can solve problems such as increasing the difficulty of solvent recovery, retention of trimethylhydroquinone, and affecting product quality, so as to reduce solvent Effects of recovery loss, cycle shortening, and high product yield

Active Publication Date: 2013-01-30
NANTONG BAISHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] After the above-mentioned catalytic hydrogenation reaction is complete, the catalyst is filtered out, and the crystals can be precipitated directly after dilution with deionized water, but some trimethylhydroquinone remains in the solvent, which not only reduces the yield but also increases the difficulty of solvent recovery
At the same time, if you want to recover the solvent completely, it will affect the quality of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 30 g of trimethylbenzoquinone, 250 g of ethyl acetate, and 3 g of skeleton nickel into the hydrogenation kettle. Introduce nitrogen for 2 replacements, hydrogen for 2 replacements, start stirring and heating, and when the temperature reaches 50°C, introduce hydrogen to control the reaction pressure to 1.0 MPa for hydrogenation reaction. When the pressure does not drop, the reaction basically ends. Continue the heat preservation reaction for 1 hour, and the reaction is completed. The reaction solution was heated and filtered at 50° C., and 100 g of water was added to the filtrate, and the azeotropic distillation was carried out under normal pressure to recover ethyl acetate, and the water was returned to the material. Stop after evaporating ethyl acetate, cool down to 80°C, add 0.6g of sodium hydrosulfite, keep warm at 80°C for 0.5 hours, cool down to 30°C, and filter. The wet product was dried at 80°C to obtain 28.8 g of trimethylhydroquinone with a content of 99.6...

Embodiment 2

[0030] Add 30 g of trimethylbenzoquinone, 250 g of butyl acetate, and 3 g of framework nickel into the hydrogenation kettle. Nitrogen was passed through for replacement twice, and hydrogen was replaced twice. Turn on stirring and heating, and when the temperature reaches 50° C., hydrogen gas is introduced to control the reaction pressure to 1.0 MPa to carry out the hydrogenation reaction. When the pressure does not drop, the reaction basically ends. Continue the heat preservation reaction for 1 hour, and the reaction is completed. The reaction solution was heated and filtered at 50° C., and 100 g of water was added to the filtrate, followed by azeotropic distillation under normal pressure to recover butyl acetate. The water returns to the material again, and the butyl acetate is evaporated to stop. Cool down to 80°C, add 0.6g of sodium hydroquinone, keep warm at 80°C for 0.5 hours, cool down to 30°C, filter, and dry the wet product at 80°C to obtain 28.6g of trimethylhydroqu...

Embodiment 3

[0032] Add 30 g of trimethylbenzoquinone, 250 g of isobutyl acetate, and 3 g of skeleton nickel into the hydrogenation kettle. Nitrogen was passed through for replacement twice, and hydrogen was replaced twice. Turn on stirring and heating, and when the temperature reaches 50° C., hydrogen gas is introduced to control the reaction pressure to 1.0 MPa to carry out the hydrogenation reaction. When the pressure does not drop, the reaction basically ends. Continue the heat preservation reaction for 1 hour, and the reaction is complete. The reaction liquid was heated and filtered at 50° C., and 100 g of water was added to the filtrate, followed by azeotropic distillation under normal pressure to recover isobutyl acetate. Water returns to the material again, steams the isobutyl acetate and stops, cools down to 80°C, adds 0.6g of hydrosulfite, keeps at 80°C for 0.5 hour, cools down to 30°C, filters, and dries the wet product at 80°C to obtain three Methyl hydroquinone 29.2g, the co...

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PUM

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Abstract

The invention discloses a preparation method of trimethyl hydroquinone, which comprises the following steps: adding 2,3,5-trimethyl benzoquinone, solvent, and Raney catalyst into a hydrogenation kettle to react, filtering, and drying to obtain the trimethyl hydroquinone product. The invention has the advantages of low raw material cost and simple operating procedure, shortens the period, reduces the solvent recovery loss, and enhances the yield and quality of the product.

Description

technical field [0001] The invention relates to a preparation method of trimethylhydroquinone. Background technique [0002] Trimethylhydroquinone (TMHQ) is the abbreviation of 2,3,5-trimethylhydroquinone, also known as 2,3,5-trimethylhydroquinone, which is an important intermediate for the synthesis of vitamin E (Ve). , can also be used as an antioxidant for various substances. Ve is a commonly used drug and nutritional health product. It has become the most widely used vitamin in the international market and has a large production and sales volume. Together with Vc and Va, it has become the three pillar products of the vitamin series and has a broad market prospect. In the world vitamin market, Ve is the variety with the fastest growing demand and sales. Over the years, global sales have been increasing at a rate of 10% every year. In the entire Ve market, synthetic Ve accounts for about 80% of the market share. [0003] The industrial synthesis of trimethylhydroquinone ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/08C07C37/07
Inventor 张天永袁仲飞尹观许庆丰
Owner NANTONG BAISHENG CHEM
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