Continuous synthesis system and method for trimethylsilylacetylene

Abstract

The invention provides a continuous synthesis system and a continuous synthesis method of trimethylsilylacetylene. The continuous system comprises a Grignard reagent continuous preparation unit, an acetylene Grignard reagent continuous synthesis unit and a trimethylsilylacetylene continuous preparation device, wherein the Grignard reagent continuous preparation unit is provided with a first feeding port and a Grignard reagent outlet; the acetylene Grignard reagent continuous synthesis unit is provided with a Grignard reagent inlet, an acetylene solution inlet and an acetylene Grignard reagentoutlet, and the Grignard reagent inlet is communicated with the Grignard reagent outlet through a Grignard reagent transfer pipe; the trimethylsilylacetylene continuous preparation device is providedwith a trimethylhalosilane inlet, an acetylene Grignard reagent inlet and a trimethylsilylacetylene outlet, the acetylene Grignard reagent inlet is communicated with the acetylene Grignard reagent outlet through an acetylene Grignard reagent transfer pipe. By adopting the continuous synthesis system for preparing trimethylsilylacetylene, the production cost can be reduced, the period can be shortened, and safety of the whole process can also be improved.

Description

technical field [0001] The invention relates to the field of synthesis of organic intermediates, in particular to a continuous synthesis system and a continuous synthesis method of trimethylsilylacetylene. Background technique [0002] Trimethylsilylacetylene is a very important intermediate in organic synthesis and one of the important silicon-based chemical raw materials; it is also an important alkynylation reagent in the preparation of various monoalkyne and polyalkyne is an essential synthetic unit. In addition, trimethylsilylacetylene has been widely used in heterocyclic chemistry, carbon-carbon coupling, drug synthesis, catalytic chemistry and materials industry. According to existing literature reports, the synthesis of trimethylsilylacetylene mostly adopts a batch synthesis process, which is mainly divided into the following stages: [0003] (1) Preparation of Grignard reagent 2: Preparation of halogenated hydrocarbon 1 and metal magnesium; (2) Preparation of acet...

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Problems solved by technology

[0008] 1. The Grignard reaction usually releases a large amount of heat, and it is necessary to control the rate of addition of halogenated hydrocarbons to control the heat release of the reaction. The production cycle of Grignard reagents prepared by batch reactions is long

[0009] 2. A large amount of flammable metal magnesium needs to be added to the reaction kettle in advance, and the residual magnesium chips need to be cleaned after the reaction, which increases the potential risk of operation and the risk of reaction amplification

[0010] 3. Grignard reagents are usually sensitive to air and water. If a large amount of Grignard reagents cannot be used in a batch reaction, storage risks will be increased and storage costs will be increased.

[0011] 4. Dissolve acetylene in batches. The acetylene solution needs to be stored at low temperature in the reactor, but when disturbed (such as stirring) or heated up, a large amount of acetylene gas may be released, which increases the risk in the production process and increases the acetylene gas. Loss

[0013] 6. In order to control impurities, it needs to be added dropwise quickly when adding trimethylchlorosilane. The larger the reaction scale, the longer the feeding time will be, which limits the scale-up

[0014] 7. The operation requires independent production time, so the complete batch production time of trimethylsilyl acetylene is longer

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