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Preparation method of lithium trimethylsilanolate

A technology of lithium trimethylsiliconate and hexamethyldisiloxane is applied in the field of preparation of lithium trimethylsiliconate, can solve problems such as high price, and achieve the effects of cheap raw materials, simple operation and simple post-processing

Active Publication Date: 2014-03-12
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such catalysts mainly include n-butyllithium, isobutyllithium and lithium trimethylsiliconate, among which the use of butyllithium and isobutyllithium to prepare block polysiloxane or single-end functional group polysiloxane is expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 250ml four-neck flask equipped with a water separator, serpentine condenser, and mechanical stirring, put 4.2g of lithium hydroxide raw material (LiOH·H 2 O), 16.6g hexamethyldisiloxane, 40g cyclohexane and 50g absolute ethanol, heated to solvent reflux, N 2 The reaction was carried out under protection for 35 hours, and vigorous stirring was maintained during the reaction, and the stirring speed was 120 rpm. Naturally cool to room temperature after the reaction, filter, take the solid as lithium trimethylsiliconate, dry at 0.1 MPa, 80°C for 2.5 hours, and obtain 8.9 g white solid lithium trimethylsiliconate product after cooling, with a yield of 93%. Sealed and filled with N 2 save.

Embodiment 2

[0020] Put 12.6g of lithium hydroxide LiOH·H in a 250ml four-neck flask equipped with water separator, serpentine condenser and mechanical stirring 2 O, 40g hexamethyldisiloxane, 60g cyclohexane and 60g absolute ethanol, heated to solvent reflux, N 2 React under protection for 27 hours. Maintain vigorous stirring during the reaction, and the stirring speed is 120 rpm. After the reaction was completed, it was naturally cooled to room temperature, filtered, and the obtained solid was lithium trimethylsiliconate, dried at 0.1 MPa and 80°C for 3 hours, and 26 g of white lithium trimethylsiliconate solid product was obtained after cooling, with a yield of 90%. Sealed and filled with N 2 save.

Embodiment 3

[0022] Put 4.2g lithium hydroxide LiOH·H 2 O, 16g hexamethyldisiloxane, 20g cyclohexane and 30g absolute ethanol, heated to solvent reflux, N 2 React under protection for 30 hours. Stirring was maintained during the reaction, and the stirring speed was 100 rpm. Naturally cool to room temperature after the reaction, filter, the obtained solid is lithium trimethylsiliconate, dry at 0.1MPa, 80°C for 3.5 hours, after cooling, 7.7g of white lithium trimethylsiliconate solid product is obtained, the yield is 80.2% . Sealed and filled with N 2 save.

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PUM

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Abstract

The invention relates to a preparation method of lithium trimethylsilanolate. According to the method, lithium trimethylsilanolate is prepared through reacting a lithium hydroxide raw material with hexamethyldisiloxane under the protection of N2 with waterless ethanol, methanol or butanol and cyclohexane as a mixed solvent. The method has the characteristics of simple synthetic process, cheap and easily available raw material, and low cost. Obtained lithium trimethylsilanolate is mainly used for initiating the ring-opening polymerisation of cyclotrisiloxane as an initiator to prepare block polysiloxanes or single-terminal function group polysiloxanes.

Description

technical field [0001] The invention relates to a preparation method of lithium trimethylsiliconate, which belongs to the technical field of synthesis of lithium compounds. Background technique [0002] Among the catalysts used in the preparation of polysiloxane, alkali metal compounds such as hydroxides of potassium, sodium, and lithium, and lithium-based compounds can only open cyclotrisiloxane when polysiloxane is prepared by ring-opening polymerization. The siloxane bond in the oxane, but not the Si-O-Si bond in the linear polysiloxane, is suitable for the preparation of block polysiloxane or single-end functional group polysiloxane. Such catalysts mainly include n-butyllithium, isobutyllithium and lithium trimethylsilanolate, among which the use of butyllithium and isobutyllithium to prepare block polysiloxane or single-end functional group polysiloxane is expensive . Therefore, the research and development of lithium trimethylsiliconate with simple synthesis process,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 冯圣玉谭景林马德鹏张长桥
Owner SHANDONG UNIV
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