Method for continuously and quickly preparing propargyl alcohol by using micro-reactor

A micro-reactor, propargyl alcohol technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, preparation of hydroxyl compounds, etc., can solve the problems of harsh reaction conditions and inconvenient operation

Inactive Publication Date: 2020-10-09
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, metal reagents such as alkylzinc and butyllithium are extremely sensitive to water, and the water content of the reaction system needs to be strictly controlled. The reagents, solvents, and utensils required for the reaction must be strictly dried without water, so the reaction conditions are harsh and the operation is inconvenient.
At present, the industrial production of propynyl alcohol basically adopts the Reppe process. Because the process uses a large amount of acetylene gas and flammable and explosive acetylene copper catalyst, the pressure of acetylene reaches 2 MPa, and safety issues have always plagued the process. main problem
At present, utilize microreactor to prepare the method for propynyl alcohol and there is no report yet

Method used

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  • Method for continuously and quickly preparing propargyl alcohol by using micro-reactor

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Experimental program
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Effect test

Embodiment 1

[0021] A kind of method utilizing microreactor to prepare propargyl alcohol continuously and rapidly, its main steps are as follows:

[0022] Under anhydrous and oxygen-free conditions, add 3.0 g metallic magnesium, 1.2 g elemental iodine and 20 mL anhydrous ether into the reactor, start stirring after the elemental iodine dissolves, and slowly add 5.0 mL ethyl bromide dropwise at a rate to maintain It is advisable for the liquid to boil, and after the dropwise addition, heat to 60 o C was refluxed for 60 min to obtain ethyl magnesium bromide; then as flow process figure 1 As shown, acetylmagnesium bromide and acetylene gas are respectively injected into the micro-mixer D1 (T-type tee, inner diameter: 0.021 mm) by the pump A and the gas controller C1 according to the molar ratio of 1:1.2. Microreactor E1 (inner diameter: 0.1 mm) at -20 o Under the condition of C, the reaction was carried out for 10 min, and the acetylene magnesium bromide was obtained through the Grignard e...

Embodiment 2

[0024] A kind of method utilizing microreactor to prepare propargyl alcohol continuously and rapidly, its main steps are as follows:

[0025] Under anhydrous and oxygen-free conditions, add 3.0 g metallic magnesium, 1.2 g elemental iodine and 20 mL anhydrous ether to the reactor. After the elemental iodine dissolves, start stirring and slowly add 5 mL vinyl iodide dropwise at a rate to maintain It is advisable for the liquid to boil, and after the dropwise addition, heat to 80 o C was refluxed for 120 min to obtain a mixed solution of vinylmagnesium iodide and ether; then, as shown in the figure, vinylmagnesium iodide and acetylene gas were respectively injected into micro-mixer D1 by pump A and gas controller C1 according to the molar ratio of 1:0.8 After mixing in the medium (T-type tee, inner diameter: 0.1 mm), it enters the microchannel reactor E1 (inner diameter: 1 mm), at 20 o Under the condition of C, it was reacted for 3 minutes, and ethynylmagnesium iodide was obtain...

Embodiment 3

[0027] A kind of method utilizing microreactor to prepare propargyl alcohol continuously and rapidly, its main steps are as follows:

[0028] Under anhydrous and oxygen-free conditions, add 3.0 g metal magnesium, 1.2 g elemental iodine and 20 mL tetrahydrofuran into the reactor, start stirring after the elemental iodine dissolves and slowly add 5 mL ethyl chloride dropwise at a rate to maintain the liquid It is advisable to boil, and after the dropwise addition, heat to 100 o C was refluxed for 180 min to obtain a mixed solution of ethyl magnesium chloride and ether; then, as shown in the figure, the ethyl magnesium chloride and acetylene gas were respectively injected into the micro-mixer D1 by the pump A and the gas controller C1 according to the molar ratio of 1:1.5 ( T-type tee, inner diameter: 10 mm) mixed in the microchannel reactor E1 (inner diameter: 10 mm), at 40 o Under the condition of C, the reaction was carried out for 60 s, and the ethynylmagnesium chloride was ...

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Abstract

The invention discloses a method for continuously and quickly preparing propargyl alcohol by using a micro-reactor. The preparation method comprises the following steps: firstly, under anhydrous and anaerobic conditions, adding magnesium metal, elemental iodine and a solvent into a reactor, uniformly stirring the components, dropwise adding halogenated hydrocarbon, continuously stirring the components, and reacting to obtain a hydrocarbyl magnesium halide Grignard reagent; in a micro-reactor, with prepared alkyl magnesium halide and acetylene as raw materials, carrying out a Grignard exchangereaction under a continuous flowing condition to obtain ethynyl magnesium halide; and carrying out nucleophilic addition reaction on acetenyl magnesium halide and formaldehyde serving as raw materialsunder a continuous flowing condition to prepare propargyl alcohol. The method has the characteristics of rapid and continuous preparation of propargyl alcohol, simple operation, continuous and controllable process, mild conditions, and realization of industrialization.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for rapidly preparing propynyl alcohol by using a microreactor. Background technique [0002] Propargyl alcohol is a key intermediate widely used in medicine, pesticides, electroplating and resin industries, and is mainly used in the preparation of pharmaceutical sulfadiazine, fosfomycin drugs, pesticide clofenac and electroplating nickel plating brightener, etc. (CN 109369328 A) . At the same time, the two flexible functional groups, alkynyl and hydroxyl, can be transformed through functional groups to have great potential application value in molecular diversity. Proynyl alcohol can be prepared by the addition reaction of terminal alkynes to aldehydes or ketones. The reaction process is generally through the reaction of active metal reagents such as alkyl zinc and butyl lithium with terminal alkynes to form alkynyl zinc or alkynyl lithium. Reagents, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/42C07C33/042C07F3/02B01J19/00
CPCC07C29/42C07F3/02B01J19/0093C07C33/042
Inventor 邓秋林黄晓枫
Owner SOUTHWEAT UNIV OF SCI & TECH
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