Preparation method of glycerinum dimethyl ether acetate
A technology of glyceryl dimethyl ether acetate and dimethyl ether acetate, which is applied in the field of preparation of glyceryl dimethyl ether acetate, can solve problems such as explosive steam/air mixture, and achieves high yield, high safety and high quality Effect
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[0020] The present invention is a kind of preparation method of glycerol dimethyl ether acetate, mainly comprises the following steps:
[0021] S1, esterification, using glycerin and acetic acid as raw materials, the product glycerol monoacetate is obtained through the catalyzed reaction of a sulfonic acid catalyst;
[0022] S2. Methylation, using glycerol monoacetate and methyl iodide obtained in the step S1 as raw materials, using a phase transfer catalyst to catalyze the reaction in an alkaline environment to obtain the product glycerol dimethyl ether acetate.
Embodiment 1
[0024] Esterification reaction
[0025] Add 9.2kg of glycerol and 3kg of cyclohexane as raw material for esterification into a 30L normal-pressure reactor. The esterification reaction is a reversible reaction and will generate water. separated from the system. Substances that can be used as water-carrying agents must react with water to produce azeotropes to make water easier to be distilled, and the solubility in water is very small, and this program uses cyclohexane as the water-carrying agent. In addition, p-toluenesulfonic acid is also added in the reactor as a catalyst for the esterification reaction, and the reactor is heated to 60°C as the reaction temperature, and then 6 kg of acetic acid, another esterification raw material, is gradually added dropwise to the reactor to make it occur. Esterification produces glycerol monoacetate and water. And the reaction can utilize the reflux system with water separator at the same time, and the water phase of the lower layer is ...
Embodiment 2
[0034] Esterification reaction
[0035] Add 9.2 kg of glycerin and 3 kg of butanone as a water-carrying agent into a 30L normal-pressure reactor. The esterification reaction is a reversible reaction and will generate water. In order to improve the conversion rate, the water-carrying agent can be used to remove water from the reaction system separated out. Substances that can be used as water-carrying agents must react with water to produce azeotropes to make water easier to be distilled, and the solubility in water is very small, and this program uses cyclohexane as the water-carrying agent. In addition, methanesulfonic acid is also added in the reaction kettle as a catalyst for the esterification reaction, and the reaction kettle is heated to 80° C. as the reaction temperature, and then 6 kg of another esterification raw material acetic acid is gradually added dropwise to the reaction kettle to make it occur. Esterification produces glycerol monoacetate and water. And the r...
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