Method for preparing alpha-ethyl furan methanol

A technology of ethyl furan methanol and tetrahydrofuran, applied in the chemical industry, can solve problems such as turbidity, loss, and freezing, and achieve the effects of stable and reliable process, high product yield and purity, and low cost

Active Publication Date: 2016-07-27
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

However, it is not easy to control the clarification point in many reactions, especially in industrial production, it is impossible to clearly distinguish whether the clarification layer has been clarified in the inner viewing hole
Once the ammonium chloride solution is added too much, the reaction system will turn turbid again, or even become frozen. At this time, a large amount of organic solvent must be added many times, and the product can only be obtained after repeated extractions, resulting in huge losses.
The same is true for the reaction of furfuryl alcohol Grignard reagent through hydrolysis of saturated ammonium chloride aqueous solution to obtain α-ethylfuranmethanol. At the same time, there are side reactions such as Wutz reaction, disproportionation reaction and its reaction with active hydrogen compounds or oxygen. , and the by-product basic magnesium chloride is a solid powder precipitate, which will take away the α-ethylfuran methanol solution, and the solid-liquid separation effect is not good

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, the preparation method of α-ethylfuran methanol of the present invention

[0024] Step 1, Grignard-addition reaction:

[0025] A1. Add toluene-tetrahydrofuran mixed solvent, 1153.0kg furfural and 851.7kg chloroethane into the header tank and stir evenly to obtain material 1. After the reaction of material 1 is complete, cool it down to 43°C with cold water;

[0026] A2. Add 288.0kg of magnesium chips, toluene-tetrahydrofuran mixed solvent and 17.4kg of bromoethane into the reaction kettle, heat to 35°C, then open the head tank and add the materials dropwise into the reaction kettle for reaction, cool down with cold water to keep the reaction The temperature is 45°C, and the dropwise addition is controlled within 3 hours to generate furfuryl Grignard reagent; check the reaction kettle, the reaction of magnesium chips is complete, and there is no residue.

[0027] Step 2, hydrolysis reaction:

[0028] B1. Transfer the generated furfuryl Grignard reagent to...

Embodiment 2

[0034] Embodiment 2, the preparation method of α-ethylfuran methanol of the present invention

[0035] Step 1, Grignard-addition reaction:

[0036] A1. Add toluene-tetrahydrofuran mixed solvent, 1153.0kg furfural and 851.7kg chloroethane into the header tank and stir evenly to obtain material 1. After the reaction of material 1 is complete, pass cold water to cool down to 47°C;

[0037] A2. Add 288.0kg of magnesium chips, toluene-tetrahydrofuran mixed solvent and 16.3kg of bromoethane into the reaction kettle, heat it to 45°C, then open the high level tank and drop the materials into the reaction kettle for a reaction, pass cold water to cool down, and keep the reaction The temperature is 55°C, and the dropwise addition is controlled within 2 hours to generate furfuryl Grignard reagent; check the reaction kettle, the reaction of magnesium chips is complete, and there is no residue.

[0038] Step 2, hydrolysis reaction:

[0039] B1. Transfer the generated furfuryl Grignard reag...

Embodiment 3

[0045] Embodiment 3, the preparation method of α-ethylfuranmethanol of the present invention

[0046] Step 1, Grignard-addition reaction:

[0047] A1. Add toluene-tetrahydrofuran mixed solvent, 1153.0kg furfural and 851.7kg chloroethane into the header tank and stir evenly to obtain material 1. After the reaction of material 1 is complete, pass cold water to cool down to 45°C;

[0048] A2. Add 288.0kg of magnesium chips, toluene-tetrahydrofuran mixed solvent and 16.8kg of bromoethane into the reaction kettle, heat it to 40°C, then open the high level tank and drop the materials into the reaction kettle for reaction, cool down with cold water, and keep the reaction The temperature is 50°C, and the dropwise addition is controlled within 2.5 hours to generate furfuryl Grignard reagent; check the reaction kettle, the reaction of magnesium chips is complete, and there is no residue.

[0049] Step 2, hydrolysis reaction:

[0050] B1. Transfer the generated furfuryl Grignard reagen...

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PUM

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Abstract

The invention belongs to the technical field of chemical engineering, and particularly relates to a method for preparing alpha-ethyl furan methanol.The method comprises the first step of a Grignard-addition reaction, wherein a methylbenzene-tetrahydrofuran mixed solvent, furfural and chloroethane are added into a head tank, magnesium chips, the methylbenzene-tetrahydrofuran mixed solvent and bromoethane are added into a reaction still, heating is carried out, then the head tank is opened, materials are dropwise added into the reaction still for reacting, the temperature is kept at 45 DEG C to 55 DEG C, and after the materials are dropwise added, a furfuryl Grignard reagent is generated; the second step of a hydrolysis reaction, wherein a hydrolysis agent is dropwise added to the furfuryl Grignard reagent and stirred, the hydrolysis agent is dropwise added till the system is clear, the temperature is controlled to range from 15 DEG C to 30 DEG C, an alpha-ethyl furan methanol solution is obtained through filtering and is distilled at vacuum negative pressure, and alpha-ethyl furan methanol is obtained.According to the method, the solvent, the material proportion and other parameters are optimized, production cost is reduced, and the purity and yield of alpha-ethyl furan methanol are improved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of α-ethylfuranmethanol. Background technique [0002] α-Ethylfuranmethanol is the raw material intermediate of the chemical synthesis method of ethyl maltol. It is usually prepared by Grignard reaction to prepare Grignard reagent, and then it is prepared by addition and hydrolysis of furfural. The Grignard reagent is prepared under the following conditions, and the Grignard reagent is added with furfural at low temperature (about 0°C), and then hydrolyzed to obtain α-ethylfuran methanol. Special requirements, and the quality of the output product is unstable. In order to overcome the problems existing in the traditional process, Chinese patent application CN101993425A and Polish patent PL157241B1 disclose a technical scheme for preparing furfuryl alcohol Grignard reagent by one-step method, which realizes the simultaneous progress of G...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/42
CPCC07D307/42
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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