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Grignard reaction method in production of maltol

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

Active Publication Date: 2009-03-25
ANHUI JINGHE IND
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  • Claims
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Problems solved by technology

[0010] 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

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  • Grignard reaction method in production of maltol

Examples

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Embodiment 1

[0019] Example 1: In the Grignard reactor (30L Grignard reagent has been reserved), drop 60Kg of magnesium chips, seal the feeding hole, inject 1200L of anhydrous ether (or tetrahydrofuran) solvent, and then evacuate to minus 0.04-negative 0.06Mpa, then feed 40Kg of methyl chloride, (normally no steam heating is required, sometimes the moisture in the solvent is too high, you can heat it slightly to shorten the initiation time) the reaction starts automatically, the temperature of the kettle rises from about 30 degrees to about 83 degrees, and the pressure of the kettle increases from about 30 degrees to about 83 degrees. Negative 0.04Mpa rises to about 0.2Mpa. At this time, the cooling water with jacket is opened to control the temperature to be less than 80 degrees. Continue to pass in methyl chloride to react. The methyl chloride is passed to 130Kg. After half an hour of natural reaction, the cooling water can be turned on to cool down. When the temperature is lowered to abo...

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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), in particular to a Grignard reaction method therein. Background technique: [0002] Maltol (including ethyl maltol) is a broad-spectrum flavor enhancer with a pleasant burnt-sweet aroma. It 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), domestic and foreign manufacturers mainly adopt the furfural route. The production process is as follows: magnesium and halogenated alkanes are reacted to synthesize Grignard reagents in the presence of anhydrous ether or tetrahydrofuran solvent, and then the Grignard reagents are Addition with furfural, and then hydrolyzed to obtain furfuryl alcohol intermediate; the furfuryl alcohol intermediate after separation of the solvent is chlorinated with chlorine gas at low temperature in methanol aqueous solution, and the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D309/32A23L1/226A23L27/20
Inventor 杨迎春
Owner ANHUI JINGHE IND