Process for preparing lithium bis (trimethyldisilyl) amide

A technology of bistrimethyldisilazylamino and hexamethyldisilazane, which is applied in the field of preparing bistrimethyldisilazide lithium, can solve the problems of crystal precipitation, low solubility, difficult recovery, etc., and improve the Utilization rate, equipment investment savings, and the effect of improving competitiveness

Pending Publication Date: 2021-04-27
SHANGYU HUALUN CHEM
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  • Abstract
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Problems solved by technology

[0008] The problems existing in the above-mentioned existing preparation process are: adopt two-step reaction, the by-product lithium chloride needs to pass through mechanical filtration; The product solvent component (tetrahydrofuran and n-hexane) directly synthesized with n-butyllithium and hexamethyldisilazane Azeotrope) is difficult to recover in downstream products; the product solubility of mixed solvents is relatively small (up to 1.1M), and crystals will precipitate out when the concentration is high

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  • Process for preparing lithium bis (trimethyldisilyl) amide

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Embodiment Construction

[0018]A lot of specific details are set forth in the following description to fully understand the present invention, but the present invention may also employ other different embodiments thereof, and therefore, the present invention is not limited to the specific embodiments disclosed below. limit.

[0019]After the process conditions, after the start of the raw material preparation, the reactor system cooling system is installed, the inert gas pipeline is installed, and the equipment is cleaned dry, and the basic preparation of personnel training is completed.

[0020]The present invention is obtained by one-step synthesis of reaction with lithium, isoprene, hexamethyldisodisiline, tetrahydrofuran as a raw material, and the finished product is obtained. The specific parameters in each embodiment are as follows:

[0021]

[0022]By comparing the above embodiment, the final selection process condition is between the temperature -20 to -10, the reaction time is 12-16 hours, the ingredient ratio ...

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Abstract

The invention provides a process for preparing lithium bis (trimethyldisilyl) amide, which comprises the following steps of: under the protection of inert gas, adding lithium, isoprene, hexamethyldisilazane and tetrahydrofuran into a reaction vessel, carrying out one-step synthesis reaction, and preparing to obtain the finished product. The product is directly synthesized by adopting a one-step method, the link of producing the n-butyllithium product is omitted, the utilization rate of metal lithium is improved, the solvent component of the product is single and only tetrahydrofuran is contained, and the solvent is simple and easy to recover; and meanwhile, the manufacturing cost is greatly saved, and the market competitiveness of the product is greatly improved.

Description

Technical field[0001]The present invention relates to the field of chemical chemical technology, and more particularly to a process for preparing a double trimethylsilicilicone-based lithium.Background technique[0002]Di (trimethylsilica) amino lithium is an organosilicon compound for aldol condensation, which is a commonly used organic base, for example, acetylenate, or prepared alcohol lithium salt.[0003]Di (trimethylsilicilicide) aminol can be used to prepare a low coordination number of complexes because of the ligand (TMS)2N- is great. Such examples have M [N (TMS)2]3(M = SC, Ti, V, Fe; TMS = (CH3)3Si)). A trimethylclycosylamine reaction was produced to produce a trim (trimethylsiliconyl) amine, wherein the nitrogen is 3, and the spatial configuration is a plane positive triangle.[0004]In the prior art 1, a synthetic method of two-step reaction is used: a metal lithium and chlorobutane are combined into n-butyllithium (2.5 m), and then in the tetrahydrofuran system and the hexam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10
CPCC07F7/10
Inventor 董暁婧崔家铭黄光亮李典正
Owner SHANGYU HUALUN CHEM
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