Method for preparing triiodomethane silicane

A technology of iodotrimethylsilane and hexamethyldisilane, which is applied in the field of halosilane preparation, can solve the problems of large copper powder consumption, reduced production cost, troublesome iodine recovery, etc., and achieves low production cost, reduced decomposition, Simple operation effect

Inactive Publication Date: 2009-12-02
WUJIANG XINYI CHEM
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Problems solved by technology

Although this method can obtain refined iodotrimethylsilane, since there are many kinds of raw materials, the recovery of iodine after the reaction is troublesome. In the refining step, the amount of copper powder is large, which is unfavorable for the reduction of production cost.

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Embodiment Construction

[0011] The specific embodiment of the present invention is described below:

[0012] A preparation method of iodotrimethylsilane, using hexamethyldisilane as raw material and refined iodine as raw material, the preparation method comprises the following steps:

[0013] (1) Put 500 kilograms of hexamethyldisilane (more than 99.5% by mass) into a 1000-liter reactor, heat up and start stirring until the liquid phase temperature of hexamethyldisilane rises to 65 degrees Celsius , add refined iodine in batches, that is, add 10kg in each batch, add the next batch after the added refined iodine has reacted, add 870 kg in total, and control the temperature of the whole feeding process within the range of 65-95 degrees Celsius. After the addition is complete, heat the reaction system to 100-110 degrees Celsius to form reflux, and allow the reaction system to reflux at this temperature for 6 hours to react the raw materials to generate crude iodotrimethylsilane;

[0014] (2) Add 7.5 kg...

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Abstract

The invention relates to a preparation method for timethylsilyl iodide. The method comprises the following steps: firstly, hexamethyldisilane is charged into a reaction vessel, and is stirred and heated, after the temperature of the hexamethyldisilane liquid is raised to 65 to 95 DEG C, refined iodine is added in batches, after the refined iodine adding is completed, a reaction system is heated to 100 to 110 DEG C to form a back flow, the back flow and the reaction are performed for 5 to 7 hours at the temperature, so that the raw material reacts to generate the crude product of iodotrimethylsilane, and the mass ratio between hexamethyldisilane and refined iodine is 1: 1.8 to 1: 1.62; secondly, the back flow is continued to the crude product of the iodotrimethylsilane after step (1), then copper powder is added, after the back flow is stopped until no color, a back flow device is changed into a distillation device, and distillation and collection are performed to obtain the timethylsilyl iodide. The mass ratio between the copper powder and the hexamethyldisilane in the raw material is 0.01 to 0.02. Through the preparation method, high-purity timethylsilyl iodide can be obtained, the operation of the method is simple and safe, and the production cost is low.

Description

technical field [0001] The invention belongs to the field of chemical product synthesis, and in particular relates to a preparation method of halosilane. Background technique [0002] In the prior art, there are more than ten kinds of synthetic methods of iodotrimethylsilane, and the more practical and industrialized synthetic methods are the synthesis of hexamethyldisiloxane, iodine and aluminum powder, hexamethyldisilane and iodine reaction. Because the raw materials of these two methods are easy to get, the process is simple, and the yield is high. However, due to the lack of one-step synthesis and reaction technology, nuclear magnetic mass spectrometry proves that there are many low-boiling impurities (tetramethylsilane and dimethyldiiodosilane). Because iodotrimethylsilane is often used to synthesize drugs such as ceftazidime, this impurity-containing product is not conducive to the synthesis of ceftazidime, and may also cause side effects after medication. The Chine...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
Inventor 钱其群
Owner WUJIANG XINYI CHEM
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