Method for synthesizing 2-methallyl alcohol through continuous hydrolysis reaction

A technology of methallyl alcohol and hydrolysis reaction, which is applied in the fields of hydrolysis preparation, chemical instruments and methods, and preparation of organic compounds, and can solve the problems of low production cost, high selectivity of 2-methallyl alcohol, and 2-methacryl alcohol. Problems such as high conversion rate of allyl chloride

Active Publication Date: 2014-02-19
SHANGHAI DUOLUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] What the present invention will solve is the low selectivity problem of 2-methallyl alcohol existing in the existing batch hydrolysis method, and a kind of method for the synthesis of 2-...

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  • Method for synthesizing 2-methallyl alcohol through continuous hydrolysis reaction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The reaction conditions are:

[0032] The raw material mixture is composed of 2-methallyl chloride in mass ratio: alkali: water: phase transfer catalyst is 1: 0.4: 3: 0.02; the alkali is sodium hydroxide, and the phase transfer catalyst is tetrabutylammonium bromide; the reaction The pressure of the reactor is 60KPa in terms of gauge pressure; the temperature of the reactor is 95° C.; the residence time in the reactor is 18 hours.

[0033] The result of the reaction is:

[0034] The conversion rate of 2-methallyl chloride is 88.9%;

[0035] The selectivity to 2-methallyl alcohol was 94.2%.

Embodiment 2

[0037] The reaction conditions are:

[0038] The raw material mixture is composed of 2-methallyl chloride in mass ratio: alkali: water: phase transfer catalyst is 1: 0.3: 1: 0.001; the base is sodium hydroxide, and the phase transfer catalyst is tetrabutylammonium bromide; the reaction The pressure of the reactor is 100KPa in terms of gauge pressure; the temperature of the reactor is 100° C.; the residence time in the reactor is 32 hours.

[0039] The result of the reaction is:

[0040] The conversion rate of 2-methallyl chloride is 90.8%;

[0041] The selectivity to 2-methallyl alcohol was 93.2%.

Embodiment 3

[0043] The reaction conditions are:

[0044] The raw material mixture is composed of 2-methallyl chloride in mass ratio: alkali: water: phase transfer catalyst is 1: 0.5: 5: 0.003; the alkali is sodium hydroxide, and the phase transfer catalyst is tetrabutylammonium bromide; the reaction The pressure of the reactor is 10KPa in terms of gauge pressure; the temperature of the reactor is 90° C.; the residence time in the reactor is 4 hours.

[0045] The result of the reaction is:

[0046] The conversion rate of 2-methallyl chloride is 89.3%;

[0047] The selectivity to 2-methallyl alcohol was 94.1%.

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Abstract

The present invention relates to a method for synthesizing 2-methallyl alcohol through a continuous hydrolysis reaction. The method comprises: 1, water, an alkali, a phase transfer catalyst and 2-methyl allyl chloride are uniformly mixed in a material preparing container to obtain a raw material mixture; 2, the raw material mixture is continuously input to the tower kettle, and evaporation is performed on the tower kettle to produce 2-methyl allyl chloride steam and the tower bottom liquid, wherein the 2-methyl allyl chloride steam rises and enters a filler bed layer; 3, a reactor circulation material and a product post-treatment material are extracted from the tower kettle, wherein the reactor circulation material is input into the tower top, then descends in the reactor, is subjected to a hydrolysis reaction with the 2-methyl allyl chloride steam at the filler bed layer, and then enters the tower bottom liquid; and 4, the unreacted 2-methyl allyl chloride rises to the tower top, and is extracted out of the reactor in the 2-methyl allyl chloride exhaust gas form, wherein the reactor pressure is 10-100 kPa, and the reactor temperature is 90-100 DEG C.

Description

technical field [0001] The invention relates to a method for synthesizing 2-methallyl alcohol by continuous hydrolysis reaction. technical background [0002] 2-Methallyl alcohol (also known as methacryl alcohol, 1-hydroxy-2-methacrylic acid, etc.) is a very important organic intermediate, which itself can undergo self-polymerization and copolymerization reactions. Using 2-methallyl alcohol as the starting material, methacrylic acid and its esters can be prepared. In addition, 2-methallyl alcohol can also form allyl esters with other organic acids. Therefore, 2-methallyl alcohol is widely used in the fields of polymer monomers and surfactants. [0003] The earliest synthesis method of 2-methallyl alcohol is to prepare 2-methallyl chloride by hydrolysis under alkaline conditions. Then there are many improved methods on this basis. [0004] US2072015 proposes hydrolysis at 120°C, catalyzed by sodium hydroxide or sodium carbonate, and 5 atmospheres. This synthesis method ne...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C29/09
CPCC07C29/124C07C33/03
Inventor 陈建华朱学文林真意舒建生徐兴建张江锋
Owner SHANGHAI DUOLUN CHEM
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