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
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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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