A device for continuously preparing Grignard reagents and a method for continuously preparing Grignard reagents using the device
A Grignard reagent and solvent technology, applied in the direction of magnesium organic compounds, etc., can solve the problems of increasing the cost of Grignard reagents, continuous production, and slow reaction speed, so as to solve the problems of initiation and heat dissipation, avoid charging or explosion, and prevent The effect of plugging valves and pipelines
Active Publication Date: 2015-08-05
SHANGHAI HEGNO PHARMA HLDG +1
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Problems solved by technology
In this method, gaseous vinyl chloride can enter the reaction kettle through a conduit, but the reaction speed is slow, and the used magnesium chips must be finer, which increases the cost of preparing the Grignard reagent.
[0005] In summary, it can be seen that the prior art for industrial preparation of Grignard reagents has not yet solved the problems of initiation and heat dissipation, and there are many shortcomings such as potential safety hazards, high preparation costs, and inability to continue production. The Industrial Production Requirements of Purity Grignard Reagent
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[0065] use figure 1 The device shown prepares the Grignard reagent, wherein the material of the bubbling sludge bed reactor used is stainless steel, the diameter is 45cm, the length is 135cm, and the height-diameter ratio is 30; the length of the lower section insulation layer is 105cm, and the upper section insulation layer length is 30cm ; The calculated total bed volume (effective reaction volume) is 1670ml, which can be filled with 1970g of magnesium particles, and the bed can be filled with a liquid volume of 700ml.
[0066] a) prepare a mother liquor with a concentration of 5wt% in a solvent-raw material mixing vessel;
[0067] b) Filling with magnesium chips
[0068] Under the protection of inert gas, 1970 g of magnesium particles were added into the bed body of the three-phase bubbling slurry bed reactor through the magnesium feeding bin;
[0069] c) Initiating a reaction
[0070] Heat the reactor to make the temperature in the reactor reach 50°C, keep warm for late...
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Abstract
The invention discloses a device for the continuous preparation of a Grignard reagent and a method for the continuous preparation of the Grignard reagent through using the device. The device comprises a solvent storage container, a solvent-raw material mixing container, a raw gas storage container, a preheater, a reactor, a magnesium adding bin, a gas-liquid separator, a Grignard reagent reception container and a tail gas recovery apparatus, wherein the reactor adopts a three-phase bubble slurry column reactor. A purpose of the continuous preparation of the Grignard reagent can be realized through using the device of the invention, and initiation and heat radiation problems of a Grignard reaction can be effectively solved through adopting the three-phase bubble slurry column reactor, so potential safety hazards of material rush-out, explosion and the like caused by the severe temperature rise of the Grignard reaction can be effectively avoided, the obstruction of valves and pipelines by magnesium shreds can be prevented, and the high purity Grignard reagent can be obtained; and the tail gas recovery apparatus is arranged in the invention to absorb and recycle tail gases, so the cost is saved, and the environmental pollution is reduced, thereby cleaning and environmental protection requirements of the preparation of the Grignard reagent are realized.
Description
technical field [0001] The invention relates to a device for continuously preparing Grignard reagents and a method for continuously preparing Grignard reagents using the device, belonging to the technical field of chemical reagent preparation. Background technique [0002] There are also many literatures on the application of Grignard reaction principle in the synthesis of various organic compounds. Initiation and heat dissipation are the key links in the industrial synthesis of Grignard reagents from gaseous halogenated hydrocarbons. The method proposed in the Chinese patent document CN200510025651.7 is to first prepare a small amount of Grignard reagent in the laboratory, and then add it to the reaction kettle to initiate the reaction; the Chinese patent document CN200410051433.6 proposes to use ultrasonic waves to initiate the reaction; proposed to initiate the reaction by microwave irradiation. There are obvious defects in the above initiation methods. Ultrasonic waves...
Claims
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IPC IPC(8): C07F3/02
Inventor 刘德铭鲁向阳王志军
Owner SHANGHAI HEGNO PHARMA HLDG