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Disiloxane compound terminated by trialkyl silica ethyl and alkyne enol and method for preparing same

A technology of alkylsilylethyl and disiloxane, which is applied in the direction of silicon organic compounds, botanical equipment and methods, non-ionic surface active compounds, etc., and can solve problems such as the instability of trisiloxane compounds

Inactive Publication Date: 2009-10-14
HUAIAN KAIYUE TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, trisiloxane compounds can only be used in a narrow range of pH 6-8. If the pH value exceeds this range, trisiloxane compounds are unstable and easy to decompose rapidly.

Method used

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  • Disiloxane compound terminated by trialkyl silica ethyl and alkyne enol and method for preparing same
  • Disiloxane compound terminated by trialkyl silica ethyl and alkyne enol and method for preparing same
  • Disiloxane compound terminated by trialkyl silica ethyl and alkyne enol and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of Trimethylsilylethyltetramethylhydrogendisiloxane (Intermediate 1):

[0030] Add tetramethyldisiloxane 103.2g in a 500 milliliter bottom four-neck round bottom flask with electric heating, Wilkinson catalyst ((PPh 3 ) 3 RhCl) 200ppm, under reflux and condensing, stir with nitrogen gas and heat up to 60°C, add 51.2g of trimethylvinylsilane dropwise at a rate of 1g / min at a reaction temperature of ≤70°C through a dropping funnel, and maintain at 65°C after the addition is complete After the reaction was completed for 1 hour, the product was distilled under reduced pressure (30 mmHg) under vacuum conditions to obtain 100 g of the target product.

[0031] Molecular structure of intermediate 1:

[0032]

Embodiment 2

[0034] Preparation of tert-butyldimethylsilylethyltetramethylhydrogendisiloxane (Intermediate 2):

[0035] Add tetramethyldisiloxane 134g, Wilkinson catalyst ((PPh 3 ) 3 RhCl) 200ppm, under reflux and condensing, stir with nitrogen gas and heat up to 60°C, add 142g of tert-butyldimethylvinylsilane dropwise at a reaction temperature of ≤70°C through the dropping funnel at a rate of 1g / min, after the addition is completed, the reaction temperature is 65 The reaction was maintained at ℃ for 2 hours. After the reaction was completed, the product was distilled under reduced pressure (30 mmHg) under vacuum conditions to obtain 140 g of the target product.

[0036] Molecular structure of intermediate 2:

[0037]

Embodiment 3

[0039] Preparation of isopropyldimethylsilylethyltetraethylhydrogendisiloxane (Intermediate 3):

[0040] Add tetraethylhydrogendisiloxane 190g in a 500 milliliter bottom four-neck round bottom flask with electric heating, Wilkinson catalyst ((PPh 3 ) 3 RhCl) 200ppm, under reflux and condensing, stir with nitrogen gas and heat up to 70°C, add 128g of isopropyldimethylvinylsilane dropwise at a reaction temperature of ≤80°C through a dropping funnel at a rate of 1g / min. The reaction was maintained at ℃ for 1 hour. After the reaction, the product was distilled under reduced pressure (30 mmHg) under vacuum conditions to obtain 150 g of the target product.

[0041] Molecular structure of intermediate 3:

[0042]

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PUM

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Abstract

The invention discloses a disiloxane compound terminated by trialkyl silicon ethyl and alkyne enol and a method for preparing the same. The method comprises the following steps: synthesizing a siloxane hydride intermediate from dihydro-terminated disiloxane and vinylsilane by the molar ratio of (1:1) in the presence of the Wilkinson's catalyst under the condition of hydrosilylation, wherein, the amount of the Wilkinson's catalyst is 200ppm of the mass of the dihydro-terminated disiloxane as the reactant; and synthesizing the alkyne-enol-terminated disiloxane compound from the siloxane hydrideintermediate and alkynyl-containing alkynol by the molar ratio of (1:1) in the presence of the Speier's catalyst, wherein, the amount of the Speier's catalyst is 50ppm to 1,000ppm of the total mass ofthe reactant. The disiloxane compound of the invention is alkynol-modified siloxane with the pH value range of resisting acid / alkali decomposition being 2 to 12; and the retention rate with the molarfraction being more than or equal to 50% exceeds far beyond 24 hours, wherein, the retention rate of 20% of the invention with the molar fraction being more than or equal to 50% exceeds 1 year underthe equivalent conditions.

Description

technical field [0001] The present invention relates to a siloxane compound and a preparation method thereof, in particular to a disiloxane compound terminated by trialkylsilylethyl and alkynyl enol and a preparation method thereof. Background of the invention [0002] In many application fields of special surfactants, trisiloxane compounds are currently one of the most representative types, which can relatively significantly control the wetting, expansion, penetration, and development of aqueous solutions at a very low concentration. Soaking, decontamination and other processes, so as to achieve the desired effect. However, trisiloxane compounds can only be used in a narrow range of pH 6-8, and if the pH value exceeds this range, trisiloxane compounds are unstable and easy to decompose rapidly. Contents of the invention [0003] The object of the present invention is to: provide trialkylsilyl ethyl and alkyne enol capped disiloxane compound and preparation method thereof...

Claims

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Application Information

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IPC IPC(8): C07F7/08A01N25/30C09D7/06C09D7/02A61K8/58C11D1/82C09D7/45C09D7/47
Inventor 张国杰夏树伟宋媛李桂军李桂民
Owner HUAIAN KAIYUE TECH DEV
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