Maltol separation and purification method
A purification method and maltol technology, applied in the field of maltol separation and purification, can solve the problems of maltol decomposition, difficult separation, low product yield, and high sublimation temperature, and achieves reduction of by-product waste asphalt, high separation efficiency, and high operation efficiency. low temperature effect
Active Publication Date: 2015-03-11
ANHUI JINGHE IND
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[0004] The purpose of the present invention is to solve the defects in the prior art that the low vacuum in the sublimation process leads to high sublimation temperature, resulting in partial decomposition of maltol, high difficulty in separation, and low product yield, and provides a method for separation and purification of maltol
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[0016] Such as image 3 As shown, replace the sublimation kettle with a molecular still, heat the asphalt (chlorinated hydrolyzate) in the preheater to 90°C, bring it to the molecular separator with a vacuum, open the oil temperature valve to heat up, and then slowly evacuate to 0.05 Below P, when the temperature reaches 110°C to 120°C, add 1000L of water to the crude product receiver and start separation. After 3.5 hours, the separation is completed, and then the by-products are scraped from the molecular separator with a scraper and discharged to the receiving tank and sent to the waste treatment station for processing.
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The invention relates to a maltol separation and purification method, which comprises the following steps: carrying out a grignard reaction, an addition reaction, a hydrolysis reaction, a chlorination hydrolysis reaction and a sublimation separation. The method is characterized in that a molecular distiller is adopted in the sublimation step, and maltol is distilled under the distillation vacuum degree of below 0.05P and at the temperature of 110 to 120 DEG C. According to the method, the vacuum degree is increased by controlling the molecular distiller, so that the sublimation temperature is decreased and the generation of waste asphalt as a byproduct is reduced. In addition, the high-temperature risk is avoided. Therefore, the product quality is improved, the yield is increased and the production cost is lowered.
Description
Technical field: [0001] The invention relates to a method for producing chemical spices, in particular to a method for separating and purifying maltol. Background technique: [0002] Maltol, especially ethyl maltol, is a new type of spice. The current production process is as follows: figure 1 shown. The sublimation section such as figure 2 As shown, first turn on the steam, heat the asphalt (chlorinated hydrolyzate) in the preheating kettle to 90°C, take it to the sublimation kettle with vacuum, and open the oil temperature valve to heat up. With the increase of the oil temperature, the temperature of the kettle will rise. Then slowly bring vacuum to below -0.09MP. When the temperature of the kettle reaches 110℃~120℃, in the late sublimation stage, the oil temperature is controlled above 260℃. [0003] The sublimation process in the traditional process is mainly cooled by simple air and water, and the vacuum limitation leads to a high sublimation temperature, which caus...
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IPC IPC(8): C07D309/40
Inventor 程光锦贺玉
Owner ANHUI JINGHE IND