Preparation method of vinyl ether by direct schizolysis of acetal liquid phase

A technology for alkenyl ether and acetal, which is applied in the field of direct cracking to prepare alkenyl ether, can solve the problems of difficulty in processing tar-like by-products, increase industrialization cost, low yield of alkenyl ether, etc., and achieves easy control of reaction conditions and equipment requirements. Low, simple production process effect

Inactive Publication Date: 2009-12-09
湖北新景新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But under this kind of reaction conditions, it is easy to produce a large amount of black tar-like substances, the yield of alkenyl ether is very low, and it is very difficult to handle the tar-like by-products, and some liquid phase media, such as silicon ether compounds, have higher prices, increasing Industrialization cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In a 500ml four-neck flask equipped with electric stirrer, thermometer, constant pressure funnel and condenser, add ethanol 226g, anhydrous sodium sulfate 113g, p-toluenesulfonic acid 1.2g, wherein anhydrous sodium sulfate is used as dehydrating agent, in 128g of propionaldehyde was added dropwise under stirring, and the temperature was controlled between 25-35°C. After the dropwise addition was completed and kept warm for 1 hour, 215g of 94% propionaldehyde diethyl acetal was refined to obtain. Put the refined propionaldehyde diethyl acetal into a 500ml three-neck flask equipped with a thermometer, distillation, condensation and receiving device, add 2g of catalyst p-toluenesulfonic acid, 20g of co-catalyst n-butylamine, and control the reaction temperature at 180℃~ At 200°C, the pyrolysis product was continuously distilled out with the distillation device, and the total mass of the collected liquid was 202.3g. Put the receiving liquid into a fractionation device with ...

Embodiment 2

[0017] In a 500ml four-neck flask equipped with electric stirrer, thermometer, constant pressure funnel and condenser, add ethanol 226g, anhydrous sodium sulfate 113g, p-toluenesulfonic acid 1.2g, wherein anhydrous sodium sulfate is used as dehydrating agent, in 128g of propionaldehyde was added dropwise under stirring, and the temperature was controlled between 25-35°C. After the dropwise addition was completed and kept warm for 1 hour, 215g of 94% propionaldehyde diethyl acetal was refined to obtain. Put the refined propionaldehyde diethyl acetal into a 500ml three-necked flask equipped with a thermometer, distillation, condensation and receiving device, add 0.2g of catalyst p-toluenesulfonic acid, 2g of cocatalyst n-butylamine, and control the reaction temperature at 180°C At ~200°C, the pyrolysis product was continuously distilled out with the distillation device, and the total mass of the collected pyrolysis solution was 182.7g. Put the receiving liquid into a fractionati...

Embodiment 3

[0019] In a 500ml four-neck flask equipped with electric stirrer, thermometer, constant pressure funnel and condenser, add ethanol 226g, anhydrous sodium sulfate 113g, p-toluenesulfonic acid 1.2g, wherein anhydrous sodium sulfate is used as dehydrating agent, in 128g of propionaldehyde was added dropwise under stirring, and the temperature was controlled between 25-35°C. After the dropwise addition was completed and kept warm for 1 hour, 215g of 94% propionaldehyde diethyl acetal was refined to obtain. Put the refined propionaldehyde diethyl acetal into a 500ml three-necked flask equipped with a thermometer, distillation, condensation and receiving device, add 2g of catalyst p-toluenesulfonic acid, 20g of cocatalyst di-n-butylamine, and control the reaction temperature at 180°C At ~200°C, the pyrolysis product was continuously distilled out with the distillation device, and the total mass of the collected pyrolysis solution was 192.6g. Put the receiving liquid into a fractiona...

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PUM

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Abstract

A preparation method of vinyl ether by direct schizolysis of acetal liquid phase comprises the following steps: adding dehydrant into alcohol and aldehyde under acidic condition to prepare the acetal, adding acidic catalyst into the acetal in the absence of any liquid phase medium, taking alkyl compound containing amidogen as a cocatalyst, the dosage of which is 1-10% of the acetal, and then carrying out reaction at the temperature of 180-200 DEG C to obtain a product, fractionating the obtained product to obtain the vinyl ether, wherein, the catalyst dosage is 0.1-1% of the acetal. The method dose not need high pressure, has low requirements on the equipment, can carry out schizolysis without adding any liquid phase medium, thus lowering the production cost; the temperature is within 200 DEG C, the reaction conditions are easily controlled; the production process is simple, thereby being easy to form industrial production.

Description

technical field [0001] The invention relates to a method for producing chemical products, in particular to a method for preparing alkenyl ether by directly cracking acetal as a raw material. Background technique [0002] Enyl ether is an important reactive monomer that can be directly used in industry for homopolymerization and copolymerization reactions, and is also an important intermediate in organic synthesis. However, enyl ethers cannot be synthesized by conventional methods for preparing ethers, because halogenated alkenes hardly show nucleophilic substitution activity, and enolates always exist in the form of their stable carbonyl tautomers, so enols The preparation of ethers has been one of the difficult problems in the field of organic synthesis for many years. [0003] Currently, there are mainly two methods for preparing enene ethers: one is gas-phase cracking of acetals in the presence of catalysts, which uses metals as catalysts, and cracks acetal vapors throug...

Claims

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Application Information

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IPC IPC(8): C07C41/28C07C43/15B01J31/04B01J31/02B01J27/16B01J21/02
Inventor 阎璟琪邓威王明星王贤东江柏生
Owner 湖北新景新材料有限公司
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