Grignard reaction method in production of maltol

A Grignard reaction and maltol technology, which is applied in the production field of maltol, can solve the problems of difficult operation control, long production cycle, high reaction pressure, etc., and achieve the goal of improving product yield, high equipment utilization rate, and product yield Effect

Active Publication Date: 2008-02-27
ANHUI JINGHE IND
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  • Abstract
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Problems solved by technology

[0014] The purpose of the present invention is exactly in order to overcome the reaction pressure height that exists in existing Grignard reaction step, operational control difficulty, production cycle is long, the shortcoming of low yield and proposes a kind of Grignard reaction method in the production of maltol

Method used

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  • Grignard reaction method in production of maltol

Examples

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Embodiment 1

[0023] Example 1: Put 60Kg of magnesium chips into the Grignard reaction kettle (30L of Grignard reagent has been reserved), seal the feeding hole, pour in 1200L of anhydrous ether (or tetrahydrofuran) solvent, and then vacuum to minus 0.04-minus 0.06Mpa, and then 40Kg of methyl chloride. (No steam heating is required. Sometimes the water in the solvent is too high. You can heat it slightly to shorten the initiation time.) The reaction starts on its own. The kettle temperature rises from about 30 degrees to about 83 degrees. Minus 0.04Mpa rises to about 0.2Mpa. At this time, open the jacket cooling water to control the temperature to be less than 80 degrees, continue to pass in the methyl chloride reaction, the methyl chloride is passed to 130Kg, and the natural reaction is half an hour, then the cooling water can be turned on and the temperature of the kettle is reduced. Decrease to about 30 degrees, vent and release the pressure, pass in nitrogen protection, discharge the materi...

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Abstract

The invention discloses a Graber's reacting method in the maltol manufacturing course, which comprises the following steps: a. extracting the autoclave into vacuum under -0. 04Mpa; b. aerating chloromethane to do Graber's reaction; controlling the pressure below 0. 25Mpa and temperature below 80 deg. c; c. cooling the temperature below 35 deg. c; decompressing to aerate nitrogen to protect; adding the material into another autoclave to drip furfural to do additional reaction; adopting the retained 2%-3% Graber's agent in the Graber's autoclave as the catalyst to lead Graber's reaction. The invention improves the equipment utility and receiving rate under low pressure without heating, which shortens the manufacturing time with high equipment utility.

Description

Technical field: [0001] The invention relates to a production method of maltol (including ethyl maltol), and particularly relates to a Grignard reaction method therein. Background technique: [0002] Maltol (including ethyl maltol) is a kind of general flavor enhancer with pleasant scorching sweet fragrance, which is widely used in daily chemicals, beverages, food, medicine, tobacco, wine and other fine chemical fields. [0003] For the production of maltol (including ethyl maltol), the current domestic and foreign manufacturers mainly adopt the furfural route. The production process is: magnesium and halogenated alkanes are reacted in the presence of anhydrous ether or tetrahydrofuran solvent to synthesize Grignard reagent, and then Grignard reagent It is added with furfural and then hydrolyzed to obtain furfuryl alcohol intermediate; the furfuryl alcohol intermediate after separating the solvent is chlorinated with chlorine gas in methanol aqueous solution at low temperature, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A23L1/226A23L27/20
Inventor 杨迎春
Owner ANHUI JINGHE IND
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