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A kind of preparation method of hydroxypropyl (butyl) disiloxane

A technology based on disiloxane and hydroxypropyl, which is applied in the field of synthesis of organosilicon compounds, can solve the problem of low efficiency, and achieve the effects of high yield, improved efficiency, and increased yield

Active Publication Date: 2018-05-08
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, the productive rate of this method alcoholysis reaction is 60%, and the productive rate of target product is only 51%, still not high

Method used

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  • A kind of preparation method of hydroxypropyl (butyl) disiloxane
  • A kind of preparation method of hydroxypropyl (butyl) disiloxane
  • A kind of preparation method of hydroxypropyl (butyl) disiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Embodiment 1, the preparation of 1,3-bis(hydroxypropyl)-1,1,3,3-tetramethyldisiloxane

[0061] The structural formula of 1,3-bis(hydroxypropyl)-1,1,3,3-tetramethyldisiloxane is as formula (IV):

[0062]

[0063] Including the following steps:

[0064] (1) Add 58.08g of allyl alcohol to a three-necked round-bottomed flask equipped with a spherical condenser with a drying tube, a magnet, and a T-shaped three-way piston, feed nitrogen, weigh 4.62g of sodium, and add in batches Put it into the reaction bottle, control the system temperature not to exceed 50°C, stir until all the sodium disappears, and obtain sodium allyl alcohol-allyl alcohol solution. The proton nuclear magnetic spectrum spectrogram of gained sodium allyl alcoholate-allyl alcohol solution is as follows figure 1 shown.

[0065] (2) add 200.15g normal hexane, 96.75g dimethyl hydrochlorosilane in the three-necked round-bottomed flask that is equipped with constant pressure dropping funnel, spherical con...

Embodiment 2

[0069] Embodiment 2, the preparation of 1,3-bis(hydroxybutyl)-1,1,3,3-tetramethyldisiloxane

[0070] The structural formula of 1,3-bis(hydroxybutyl)-1,1,3,3-tetramethyldisiloxane is as formula (Ⅴ):

[0071]

[0072] Including the following steps:

[0073] (1) Add 72.45g 3-buten-1-alcohol, 20.95g potassium hydroxide, 200.00g hexanaphthene in the three-necked round bottom flask that has the spherical condenser tube that has drying tube, magneton, heating system, Reflux, remove water azeotropically to obtain potassium-3-butene-1-alcohol solution.

[0074] (2) Add 175.49g of cyclohexane and 92.78g of dimethylhydrochlorosilane to a three-necked round-bottomed flask equipped with a constant-pressure dropping funnel, a spherical condenser with a drying tube, a magneton, and a T-shaped three-way piston. , into the dry argon, the gas rate of 0.3m 3 / h, put the system in an ice-water bath, add the potassium butylate-3-buten-1-ol solution dropwise to the system at a rate of 2ml / min...

Embodiment 3

[0077] Embodiment 3, the preparation of 1,3-bis(hydroxypropyl)-1,1,3,3-tetramethyldisiloxane

[0078] The structural formula of 1,3-bis(hydroxypropyl)-1,1,3,3-tetramethyldisiloxane is as formula (IV),

[0079] Including the following steps:

[0080] (1) Add 58.08g of allyl alcohol into a three-necked round-bottomed flask equipped with a spherical condenser with a drying tube, a magnet, and a T-shaped three-way piston, feed nitrogen, weigh 4.71g of sodium, and add in batches Put it into the reaction bottle, control the system temperature not to exceed 50°C, stir until all the sodium disappears, and obtain sodium allyl alcohol-allyl alcohol solution.

[0081] (2) Add 100.00 g of n-hexane, 100.00 g of xylene, and 94.96 g of xylene in a three-necked round-bottomed flask equipped with a constant-pressure dropping funnel, a spherical condenser with a drying tube, a magnet, and a T-shaped three-way piston. Base hydrochlorosilane, pass through dry nitrogen, the gas flow rate is 0.2m...

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Abstract

The present invention relates to a preparation method of hydroxypropyl (butyl) disiloxane. The steps are as follows: (1) mixing an allyl alkoxide-allyl alcohol mixed solution or an allyl alkoxide- allyl alcohol mixed solution with hydrogen chloride Silane is mixed in an organic solvent, inert gas is introduced, the reaction is stirred, distilled, and fractions are collected to obtain an alcoholysis product; (2) The hydrosilylation catalyst and cocatalyst are added to the alcoholysis product, and the reaction is stirred for 4 to 10 hours , after the reaction is completed, it is naturally cooled to room temperature; (3) the hydrochloric acid solution is added to the product obtained in step (2), and the reaction is stirred and refluxed for 5 to 12 hours. The lower layer solution is removed, the organic phase is washed with water until neutral, the organic phase is extracted with an extractant, the extractant is removed, and dried. The method of the invention has high yield of the target product, the highest yield of the alcoholysis product can reach 94.32%, and the highest yield of the addition-hydrolyzed product can reach 89.58%.

Description

technical field [0001] The invention relates to a method for preparing hydroxypropyl (butyl) disiloxane by using hydrochlorosilane as a raw material, and belongs to the technical field of organosilicon compound synthesis. Background technique [0002] Hydroxypropyl (butyl) disiloxane is a raw material for the production of many important materials such as special polysiloxanes, silicone rubbers, and silicone-modified polymers. Its preparation method is mainly hydroxyl protection method, that is, hydrogen-containing disiloxane and allyl alcohol or 3-butene-1-alcohol are prepared through hydrosilylation reaction. However, in the reaction, hexamethyldisilazane and trimethylchlorosilane are usually used as protective agents to protect the hydroxyl group of the alcohol, the process is complicated, the operation is difficult, and the yield is not high. [0003] In addition, hydroxypropyl (butyl) disiloxane can also be prepared by the method of hydrochlorosilane alcoholysis-hydros...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 张洁张玉晗庞博冯圣玉
Owner SHANDONG UNIV
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