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Method for continuously preparing 2-methylallyl alcohol

A technology of methallyl alcohol and methallyl chloride, which is applied in the field of continuous preparation of 2-methallyl alcohol, can solve problems such as troublesome operation, achieve less by-products, high reaction selectivity, and high yield high effect

Active Publication Date: 2018-06-22
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, phase transfer catalysts are involved in the esterification reaction of this process, and the esterification reaction is intermittent, and the saponification reaction is carried out after the product is processed. The two-step reaction is completely separated, and the operation is troublesome.

Method used

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  • Method for continuously preparing 2-methylallyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] exist figure 1 Shown total volume is 6 stages of stirring series reactor 1 bottoms of 500L with 136Kg / hour to pass through the sodium acetate solution (containing sodium acetate 36.0%, sodium chloride 7.5%, about 75 ℃ of temperature) that reaches balance through continuous mechanical application, simultaneously Pass into MAC with 9.05Kg / hour; Pass into the sodium hydroxide solution (containing sodium hydroxide 41%) that total amount is 9.8Kg / hour respectively in 6 stirring sections, the feeding amount of every section is controlled with pH meter (pH value is controlled at 11), at this moment, residence time is about 4 hours. At the outlet of the upper part of the reactor 1, the temperature of the reaction product is about 100° C., and the layer passes through the continuous stratifier 2. The oil layer enters the middle part of the continuous azeotropic distillation column 7, and the water layer enters the flasher 3.

[0047] Under the condition that the heat source ...

Embodiment 2

[0050] exist figure 1 Shown total volume is 10 stages of stirring series reactor 1 bottoms of 500L with 315Kg / hour to pass through the sodium acetate solution (containing sodium acetate 38.5%, sodium chloride 7.3%, about 89 ℃ of temperature) that reaches equilibrium through continuous mechanical application, simultaneously Feed MAC with 18.1Kg / hour; Feed the sodium hydroxide solution (containing sodium hydroxide 40%) that total amount is 20.0Kg / hour in 10 stirring sections respectively, the feeding amount of every section is controlled with pH meter (pH value is controlled at 10), at this moment, residence time is about 2 hours. At the outlet of the reactor 1, the temperature of the reaction product is about 110° C., and the layer passes through the continuous stratifier 2. The oil layer enters the middle part of the continuous azeotropic distillation column 7, and the water layer enters the flasher 3.

[0051] Under the condition that the heat source is provided by the re...

Embodiment 3

[0054] exist figure 1 Shown total volume is 500L 15 stages of stirred series reactor 1 bottoms with 597Kg / hour pass through the sodium acetate solution (containing sodium acetate 41.2%, sodium chloride 7.0%, about 101 ℃ of temperature) that reaches balance through continuous mechanical application, simultaneously Pass into MAC with 27.15Kg / hour; Feed in the sodium hydroxide solution (containing sodium hydroxide 39%) that total amount is 30.9Kg / hour in 15 stirring sections respectively, the feeding amount of every section is controlled with pH meter (pH value is controlled at 9), at this time, the residence time is about 1 hour. At the outlet of the reactor, the temperature of the reaction product is about 120° C., and the layer passes through the continuous stratifier 2 , the oil layer enters the middle part of the continuous azeotropic distillation column 7 , and the water layer enters the flasher 3 .

[0055] Under the condition that the heat source is provided by the re...

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Abstract

The invention relates to a method for continuously preparing 2-methylallyl alcohol. The method comprises the steps of: adopting a multi-stage series continuous stirring reactor, performing a reactionon a sodium acetate solution and 2-methylallyl chloride with sodium hydroxide to obtain 2-methylallyl alcohol directly, and performing separation after the product is collected from the upper part ofthe reactor, wherein the remaining substances, water and the sodium acetate solution, in the collected substances from the upper part of the reactor can be reused in the reactor except the desired product; meanwhile, sodium chloride produced during the reaction can be precipitated automatically by controlling high-content sodium acetate and the pH value of the reaction, and the sodium acetate mother solution can be reused in the reactor. The MAC and sodium hydroxide are adopted as raw materials, and only two kinds of products, 2-methylallyl alcohol and sodium chloride crystals, are obtained after the continuous reaction and separation are performed in the high-molar-ratio sodium acetate solution; reaction heat is applied to the step-by-step heating process of the materials, and additionalenergy is not required, so that energy consumption of the process is low, and the water in the reaction process can be applied to cyclic preparation of the sodium hydroxide solution and be added intothe reaction.

Description

technical field [0001] The invention relates to a continuous preparation method of 2-methallyl alcohol, which belongs to the technical field of organic chemical industry. Background technique [0002] 2-Methallyl alcohol (abbreviated as MAOH) is an important organic intermediate, which can be used as polymer monomer, resin and perfume, and its most important use is to synthesize methallyl polyoxyethylene ether. Methallyl polyoxyethylene ether is an important monomer for the synthesis of the fourth-generation polycarboxylate-based concrete water-reducer. Decisive. The application of methallyl polyoxyethylene ether can improve the fluidity and flow retention of the concrete mixture, reduce the slump and shrinkage, so that the polycarboxylate superplasticizer can be used more widely and more adaptable Strong, can be used in water conservancy, nuclear power engineering and other important fields. [0003] The synthesis of 2-methallyl alcohol mainly has two technological route...

Claims

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Application Information

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IPC IPC(8): C07C29/124C07C33/03C07C29/74C07C29/80
CPCC07C29/124C07C29/74C07C29/80C07C33/03
Inventor 尹红陈志荣王伟松王新荣王胜利金一丰董楠高洪军马定连
Owner ZHEJIANG UNIV
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