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Preparation method of alpha-vinyl and omega-hydroxyl siloxane oligomer

A technology of hydroxysiloxane and vinyl, which is applied in the field of α-vinyl, can solve the problems of many intermediate links in the reaction, poor stability of raw materials, and low production efficiency, and achieve good product yield, less side reactions, and safe feeding process Effect

Pending Publication Date: 2022-05-31
HUNAN UNIV OF SCI & ENG
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It effectively solves the technical problems of poor raw material stability, many reaction intermediate links, many by-products and low production efficiency in the preparation of asymmetric siloxane oligomers in the prior art.

Method used

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  • Preparation method of alpha-vinyl and omega-hydroxyl siloxane oligomer
  • Preparation method of alpha-vinyl and omega-hydroxyl siloxane oligomer
  • Preparation method of alpha-vinyl and omega-hydroxyl siloxane oligomer

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preparation example Construction

[0025] The invention provides a kind of α-vinyl, the preparation method of ω-hydroxyl siloxane oligomer, comprises the following steps:

[0026] Under vacuum conditions, dissolve the cyclic polysiloxane monomer in the solvent and mix it with the vinyl magnesium halide solution to react to generate α-vinyl, ω-hydroxyl siloxane oligomers;

[0027] Described α-vinyl, the structural formula of ω-hydroxyl siloxane oligomer is as follows:

[0028]

[0029] As a preference, where R 1 is methyl or ethyl; R 2 It is a hydrogen atom or a phenyl group; n is an integer between 2 and 4.

[0030] The structural formula of the cyclic polysiloxane monomer is as follows:

[0031]

[0032] As a preference, where R 1 is methyl or phenyl; R 2 is vinyl or -CH 2 CH 2 CF 3 ; n is 3.

[0033] Preferably, the vinylmagnesium halide solution is a vinylmagnesium bromide solution.

[0034] Preferably, the molar ratio of the cyclic polysiloxane monomer to tetrahydrofuran is 1:6-7.5.

[0035...

Embodiment 1

[0041] The preparation of the tetrahydrofuran solution of vinylmagnesium bromide, concrete operation steps are as follows:

[0042] Take 5 parts of magnesium powder, pass dry argon gas under heating conditions (65°C) for 30 minutes, add 1 part of iodine, add 7.5 parts of dry tetrahydrofuran and 4 parts of bromoethylene, stir and react at room temperature for 24 hours, the reaction solution becomes cloudy, and filtered to obtain Tetrahydrofuran solution of vinylmagnesium bromide, determine the concentration of vinylmagnesium bromide solution by titration, and set aside.

Embodiment 2

[0045] α-vinyl, ω-hydroxysiloxane oligomer preparation, the cyclic polysiloxane monomer selected in this embodiment is hexamethylcyclotrisiloxane, and the specific operation steps are as follows:

[0046] S1 Dry hexamethylcyclotrisiloxane, and dry tetrahydrofuran under sodium reflux; add 1 part of hexamethylcyclotrisiloxane to 5 parts of tetrahydrofuran, stir to dissolve it; pass dry nitrogen into it, and bubble for 15 minutes ; Then add vinylmagnesium bromide tetrahydrofuran solution containing 1 part of vinylmagnesium bromide under nitrogen protection.

[0047] S2 was heated to 70° C., stirred at constant temperature and reacted for 20 hours, then stopped stirring and cooled to room temperature.

[0048] Add saturated ammonium chloride aqueous solution at 5°C to S3, separate the layers, and take the organic phase.

[0049] S4 Vacuum distillation to obtain α-vinyl, ω-hydroxyl siloxane oligomers.

[0050] It was determined that the yield of the α-vinyl, ω-hydroxyl siloxane o...

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Abstract

The invention belongs to the technical field of organic silicon, and discloses a preparation method of an alpha-vinyl and omega-hydroxyl siloxane oligomer, which comprises the following steps: under a vacuum condition, dissolving a cyclic polysiloxane monomer in a solvent, mixing with a vinyl magnesium halide solution, and reacting to generate the alpha-vinyl and omega-hydroxyl siloxane oligomer. And a [omega]-hydroxysiloxane oligomer. According to the method, the safe and stable cyclic polysiloxane monomer is used as a raw material, so that the use of an easily-hydrolyzed silane monomer is avoided; and the method also has the advantages of simple reaction steps, few reaction byproducts, easy product separation and the like.

Description

technical field [0001] The invention relates to the technical field of organosilicon, in particular to a preparation method of α-vinyl, ω-hydroxyl siloxane oligomers. Background technique [0002] Organosilicon materials combine the properties of inorganic materials and organic materials. In addition to basic properties such as low surface tension, small viscosity-temperature coefficient, high compressibility, and high gas permeability, they also have high and low temperature resistance, electrical insulation, oxidation resistance, stability, Excellent properties such as weather resistance, flame retardant, water repellency, corrosion resistance, non-toxic and tasteless, and physiological inertness are widely used in aerospace, electrical and electronic, construction, transportation, chemical, textile, medical and other industries, among which silicone is mainly used in sealing , bonding, lubrication, surface activity, demoulding, defoaming, antifoaming, etc., so it is also ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C08G77/20C08G77/24
CPCC07F7/0878C08G77/045
Inventor 彭村覃佐东唐武飞王毅周强周军唐海珊
Owner HUNAN UNIV OF SCI & ENG
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