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Method for preparing methallyl alcohol and amide simultaneously

A technology of methallyl alcohol and methallyl carboxylate, which is applied in the field of preparation of methallyl alcohol and a series of amide compounds, can solve the problems of instability and easy polymerization of methallyl aldehyde, and achieve the reaction Effects of mild conditions and cost reduction

Active Publication Date: 2017-11-07
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantages that methacrolein is unstable and easy to polymerize

Method used

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  • Method for preparing methallyl alcohol and amide simultaneously
  • Method for preparing methallyl alcohol and amide simultaneously

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation method of embodiment 1 raw material methallyl acetate

[0023] In a 5L reaction flask, stir, and add 2000g of a 30% sodium acetate aqueous solution. Heat to about 70°C, add 100g of cuprous chloride as a catalyst, slowly add 600g of methallyl chloride dropwise, control the temperature within 70°C, after the dropwise addition of methallyl chloride is completed, slowly raise the temperature and keep reflux, Until the reflux temperature is 94°C, the reaction is over; standing for stratification, the upper layer is methallyl acetate, rectification to obtain 520g, 99% methallyl acetate, the obtained methallyl acetate HNMR 1.7ppm3H, 2.0ppm3H, 4.75ppm2H, 4.9ppm1H, 5.0ppm1H.

Embodiment 2

[0024] The preparation of embodiment 2 methallyl alcohol and formamide

[0025] Stir in a 5L reaction flask, add 2000g of methallyl formate, add 100g of basic alumina, and cool to 0°C. Ammonia gas is introduced slowly, and the temperature of the reaction system is controlled at about 0-5°C. About 350g of ammonia gas was introduced, and the gas phase detection of methallyl formate was basically consumed. Stop responding. Atmospheric distillation collected fractions at 114°C, which were 1368 g of methallyl alcohol, with a yield of 95%. The obtained methallyl alcohol HNMR 1.7ppm3H, 4.2ppm2H, 4.9ppm1H, 5.0ppm1H, 2.0ppm1H. Change vacuum distillation, collect formamide distillate 850g, yield 94.4%. Formamide HNMR 2.0 ppm 2H, 8.1 ppm 1H.

Embodiment 3

[0026] The preparation of embodiment 3 methallyl alcohol and N-methylformamide

[0027] In a 5L reaction flask, stir, add 2000g of methallyl formate, add 90g of basic alumina, and cool to 5°C. Slowly feed methylamine gas, and control the temperature of the reaction system in the range of 3-10°C. About 650g of methylamine gas was introduced, and the gas phase detection of methallyl formate was basically consumed. Stop responding. Atmospheric pressure distillation collects 114°C fraction, which is 1400g of methallyl alcohol. Distill under reduced pressure to collect 1080 g of N-methylformamide fractions.

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Abstract

A method for preparing methallyl alcohol and amide simultaneously is characterized in that methylallyl carboxylate taken as a raw material and an amine compound taken as an ammonolysis agent react under the action of a catalyst to produce methallyl alcohol and an amide compound. The methylallyl carboxylate and the amine compound taken as the ammonolysis agent are firstly adopted, and the methallyl alcohol and the amide compound are obtained under the action of the catalyst. The reaction process is a bulk reaction, no solvents are added, almost no wastewater or salt are produced, and byproduct methyl allyl ether is not produced; the defect that a large number of wastewater is produced through hydrolysis is overcome due to adoption of ammonolysis, the methallyl alcohol and the amide compound are coproduced directly by use of ammonoysis, coupling production is realized, and the cost is reduced.

Description

technical field [0001] The invention relates to a preparation method of methallyl alcohol and a series of amide compounds. In particular, it relates to a method for preparing methallyl alcohol by using methylallyl carboxylate as a raw material and ammonia gas or an organic amine as an ammonolysis agent, and simultaneously producing amides. Background technique [0002] Methallyl alcohol is an important organic intermediate, which is widely used in perfume synthesis, resin synthesis, surfactant synthesis and so on. In recent years, it has been applied to the synthesis of high-performance cement additive polycarboxylic acid macromonomers, and the market usage has increased significantly, reflecting the importance of the synthesis technology of methallyl alcohol. Amide compounds, such as formamide and dimethylamide, are raw materials for the synthesis of medicines, spices, dyes, etc., and can also be used as solvents for spinning synthetic fibers, plastic processing, polyureth...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C29/00C07C233/03C07C233/05C07C231/02
CPCC07C29/00C07C231/02C07C33/03C07C233/03C07C233/05
Inventor 张华星蒋勇军杨志杰吕海霞皮河山
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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