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Alkyl-substituted disiloxane and preparation method thereof

A technology of disiloxane and alkyl, which is applied in the field of alkyl-substituted disiloxane and its preparation, and can solve problems such as unsatisfactory use temperature and prone to gelation

Inactive Publication Date: 2012-10-17
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the commonly used polysiloxane-based synthetic oils cannot meet the requirements of use in harsh environments for a long time, and are prone to gelation; therefore, people have been looking for alternative synthetic oils with better performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Preparation of 1,2,3,1',2',3'hexaoctyldisiloxane

[0062] Magnesium chips (35 mmol, 0.840 g) were added to a three-necked flask equipped with a condenser tube, a constant pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated and nitrogen was passed three times. Add C to the constant pressure dropping funnel under nitrogen protection. 8 h 17 Br (31mmol, 5.986g) -THF (ie tetrahydrofuran) (10ml) solution, slowly drop a small amount of C 8 h 17 Br-THF solution enters the system to initiate the reaction. After the Grignard reagent in the system is stable, add SiCl to the constant pressure dropping funnel 4 (10mmol, 1.7g)-petroleum ether (5ml) solution, after the mixed solution was added dropwise within 2h, the temperature was raised to 50 o C continued to react for 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted wit...

Embodiment 2

[0065] Preparation of 1,2,3,1',2',3'hexadecyldisiloxane

[0066] Magnesium chips (35 mmol, 0.840 g) were added to a three-necked flask equipped with a condenser tube, a constant-pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated and nitrogen was passed three times. Add C to the constant pressure dropping funnel under nitrogen protection. 10 h 21 Br (31mmol, 6.851g) -THF (10ml) solution, slowly drop a small amount of C 10 h 21 Br-THF solution enters the system to initiate the reaction. After the Grignard reagent in the system is stable, add SiCl to the constant pressure dropping funnel 4 (10mmol, 1.7g)-petroleum ether (5ml) solution, after the mixed solution was added dropwise within 2h, the temperature was raised to 50 o C continued to react for 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted with petroleum ether, ...

Embodiment 3

[0071] Preparation of 1,2,3,1',2',3'hexa-dodecyldisiloxane

[0072] Magnesium chips (35 mmol, 0.840 g) were added to a three-necked flask equipped with a condenser tube, a constant-pressure dropping funnel, and a magnetic stirrer, and the reaction system was evacuated and nitrogen was passed three times. Add C to the constant pressure dropping funnel under nitrogen protection. 12 h 25 Br (31mmol, 7.726g) -THF (10ml) solution, slowly drop a small amount of C 12 h 25 Br-THF solution enters the system to initiate the reaction. After the Grignard reagent in the system is stable, add SiCl to the constant pressure dropping funnel 4 (10mmol, 1.7g)-petroleum ether (5ml) solution, after the mixed solution was added dropwise within 2h, the temperature was raised to 50 o C continued to react for 4h. A small amount of 5% dilute hydrochloric acid was added to the reaction system to stop the reaction, the organic phase was recovered, the aqueous phase was extracted with petroleum ethe...

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Abstract

The invention discloses alkyl-substituted disiloxane shown by a chemical formula (I), and a preparation method thereof. The preparation method of the compound comprises the steps that: raw materials are adopted according to a molar ratio of magnesium to bromoalkane to silicon tetrachloride of 3-3.5:3-3.3:1; magnesium is added into a reaction vessel; bromoalkane-tetrahydrofuran or an anhydrous diethyl ether solution and a silicon tetrachloride-ligroin solution are added under the protection of nitrogen gas; the mixture is subjected to a reaction for 2-6h under a temperature of 20-60 DEG C; an ammonium chloride solution or dilute hydrochloric acid is mixed into the mixture for stopping the reaction; an organic phase is separated from an aqueous phase; the aqueous phase is extracted by using an organic solvent, and the organic phases are combined; the mixture is washed by using deionized water, and is dried by using a drying agent; the material is subjected to pump-filtration; the filtrate is subjected to distillation concentration, and is dehydrated for 3-4h under a temperature of 160-260 DEG C; the material is then subjected to silica gel column chromatography, such that the alkyl-substituted disiloxane is obtained. The alkyl-substituted disiloxane provided by the invention has good thermal stability, good oxidation resistance, and high flash point. The compound is suitable to be used in hydraulic oil, diffusion pump oil, and heat conduction oil.

Description

technical field [0001] The invention belongs to an organic compound with one or more C—Si bonds, and relates to an alkyl-substituted disiloxane and a preparation method thereof. The prepared siloxane compound is especially suitable for heat-resistant and anti-oxidation medium oil. Background technique [0002] Organosilicon compounds can be used in hydraulic oil, heat transfer oil and diffusion pump oil due to their high thermal stability, oxidation resistance and high flash point. In the prior art, the commonly used polysiloxane-based synthetic oils cannot meet the requirements for use in harsh environments for a long time, and are prone to gelation; therefore, people have been looking for alternative synthetic oils with better performance. Contents of the invention [0003] The object of the present invention is to overcome the deficiencies in the prior art, and provide alkyl-substituted disiloxane and its preparation method, or alkylphenyl-substituted disiloxane and it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 杨军校刘天洋蒋道建吕欣刘彤兰琼曹志伟樊星黄亚文曹克杨海君
Owner SOUTHWEAT UNIV OF SCI & TECH
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