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Synthetic process of ethyl maltol

A technology of ethyl maltol and synthesis process, applied in the field of synthesis process of ethyl maltol, can solve the problems of low chlorination efficiency and frequent appearance of citrine, and achieve improved yield, improved chlorination efficiency, and stable process Effect

Active Publication Date: 2016-08-31
广东省肇庆香料厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems in the prior art (such as low chlorination efficiency, frequent appearance of foamy yellow crystals, low yield and purity, etc.), the invention provides a synthesis process of ethyl maltol, which effectively solves the problem of chlorine Low conversion efficiency, frequent appearance of foamy citrine and other problems, improve the yield and purity of ethyl maltol, and at the same time detailed operation steps, specific parameters, stable process, and industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1, the synthetic technique of ethyl maltol of the present invention

[0036] The first step, chlorination reaction:

[0037] a1. Add α-ethylfuranmethanol, methanol aqueous solution and polyethylene glycol with an average molecular weight of 200 to the head tank in advance, stir well and freeze to -18°C with cold brine in the jacket;

[0038] a2. Add methanol aqueous solution to the chlorination reaction kettle, stir well, and chill the jacket with cold brine to -18°C, then feed chlorine gas, and at the same time open the high level tank to add α-ethylfuran methanol mixed solution dropwise, control the chlorine gas and dripping The flow ratio of adding α-ethylfuran methanol mixed solution is 1.8L: 1kg, and the reaction temperature is controlled at -8°C to obtain a chlorinated solution; the amount of chlorine flowing during the dropwise addition is 7 / 8 of the total amount of chlorine passing, and the remaining total 1 / 8 of the chlorine flow rate is used as the...

Embodiment 2

[0049] Embodiment 2, the synthetic technique of ethyl maltol of the present invention

[0050] The first step, chlorination reaction:

[0051] a1. Add α-ethylfuranmethanol, methanol aqueous solution and polyethylene glycol with an average molecular weight of 400 to the head tank in advance, stir well and freeze to -25°C with cold brine through the jacket;

[0052] a2. Add methanol aqueous solution to the chlorination reaction kettle, stir well, and chill the jacket with cold brine to -25°C, then feed chlorine gas, and at the same time open the high-level tank to add a mixed solution of α-ethylfuran methanol dropwise, and control the flow of chlorine gas and dripping. The flow ratio of adding α-ethylfuran methanol mixed solution is 2.3L: 1kg, and the reaction temperature is controlled at -15°C to obtain a chlorinated solution; the amount of chlorine flowing during the dropwise addition is 7 / 8 of the total amount of chlorine passing, and the remaining total 1 / 8 of the chlorine ...

Embodiment 3

[0063] Embodiment 3, the synthetic technique of ethyl maltol of the present invention

[0064] The first step, chlorination reaction:

[0065] a1. Add α-ethylfuranmethanol, methanol aqueous solution and polyethylene glycol with an average molecular weight of 300 to the header tank in advance, stir well and freeze to -20°C with cold brine in the jacket;

[0066] a2. Add methanol aqueous solution to the chlorination reaction kettle, stir well and chill the jacket with cold brine to -20°C, then feed chlorine gas, and open the high level tank to add α-ethylfuran methanol mixed solution dropwise, control the chlorine gas and dripping The flow ratio of adding α-ethylfuran methanol mixed solution is 2.0L: 1kg, and the reaction temperature is controlled at -10°C to obtain a chlorinated solution; the amount of chlorine flowing during the dropwise addition is 7 / 8 of the total amount of chlorine passing, and the remaining total 1 / 8 of the chlorine flow rate is used as the amount of addi...

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Abstract

The invention belongs to the technical fields of spices and in particular relates to a synthetic process of ethyl maltol. The process comprises a chlorination reaction step, a hydrolysis rearrangement step and a sublimating and purifying step, wherein the chlorination reaction is realized by reacting alpha-ethylfuran methanol with chlorine at the flow ratio of (1.8 to 2.3L):1kg to generate a hydroxy chlorovinylketone intermediate; the hydrolysis rearrangement means that the hydroxy chlorovinylketone intermediate is hydrolyzed at the temperature of 90 to 105DEG C for 3 to 4.5 hours to obtain an ethyl maltol coarse crystal; the coarse crystal is sublimated and purified under the conditions that the temperature is 200 to 225DEG C and the pressure is 0.080 to 0.090MPa to obtain an ethyl maltol product. The synthetic process disclosed by the invention is detailed and specific in operation and is stable; the chlorinating efficiency is improved and the generation of foamed yellow crystals is controlled; meanwhile, sublimating and purifying conditions are controlled, thereby effectively improving the yield and the purity of the ethyl maltol.

Description

technical field [0001] The invention belongs to the technical field of spices, and in particular relates to a synthesis process of ethyl maltol. Background technique [0002] Ethyl maltol is a broad-spectrum aroma, aroma synergist, sweetener and bad taste masking agent, widely used in the preparation of various flavors and directly used in food, beverages, feed, cigarettes, drugs, In toothpaste and cosmetics, etc., it has a wide range of uses, a small amount of use, and significant effects. At the same time, due to the chemical activity and stable characteristics of ethyl maltol, it can also be used as antiseptic and antibacterial agent and other industrial products, so the market demand is relatively large and has an increasing trend year by year. [0003] Take α-ethyl furan methanol and chlorine as the reaction process of raw material synthetic ethyl maltol as follows: the first step chlorination reaction: α-ethyl furan methanol and chlorine react at low temperature to pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/40
CPCC07D309/40
Inventor 张翼飞阮进林韦超成郑东志简柏柳
Owner 广东省肇庆香料厂有限公司
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