Hydroxyl silicone oil and continuous preparation method thereof

A technology of hydroxysilicone oil and hexamethylcyclotrisiloxane, which is applied in the field of hydroxysilicone oil and its continuous preparation, can solve the problems of small effective surface area, low catalytic efficiency, and low conversion rate, and achieve large contact area, slow down Dehydration condensation reaction, good storage stability

Active Publication Date: 2016-07-13
GUANGZHOU DAOLIN SYNTHETIC MATERIALS CO LTD
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Problems solved by technology

[0005] The Chinese patent application number 200810105655X discloses a method for preparing low molecular weight hydroxy silicone oil, which uses perfluorosulfonic acid ion exchange resin (Nafion resin) as a catalyst to prepare low viscosity hydroxy silicone oil, although perfluorosulfonic acid resin is acidic and Concentration of 100% H 2 SO 4 It is equivalent, but because it is a perfluoropolymer without voids, the effective surface area is small, and the catalytic efficiency is not high when used as a catalyst. Therefore, the conversion rate is not high when used in continuous production

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  • Hydroxyl silicone oil and continuous preparation method thereof

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[0026] A continuous preparation method of hydroxy silicone oil, comprising the following steps:

[0027] 1) Add hexamethylcyclotrisiloxane, solvent and water into a mixing tank, stir and mix evenly, then transfer to a fluidized bed equipped with a catalyst to fully react;

[0028] 2) Adsorption filtration, ultrafiltration membrane filtration, delowering under normal pressure, delowering under reduced pressure to obtain hydroxyl silicone oil, recover solvent and unreacted low molecular compounds, and recycle after checking the content of each component.

[0029] Preferably, the molar ratio of hexamethylcyclotrisiloxane, solvent and water in step 1) is 1: (1-5): (1.2-1.5).

[0030] Preferably, the solvent in step 1) is at least one of dichloromethane, tetrahydrofuran, chloroform, acetone, and methanol.

[0031] Preferably, the catalyst in step 1) is Nafion / SiO 2 A nanocomposite material, wherein the mass fraction of Nafion is 5-40%.

[0032] Further preferably, the Nafion / SiO...

Embodiment 1

[0040] 1) Add hexamethylcyclotrisiloxane, methanol and deionized water into the mixing tank according to the molar ratio of 1:2:1.5, and stir and mix for 30 minutes;

[0041] 2) Transfer the material into a Nafion / SiO 2 Catalytic reaction at 60°C for 40 minutes in a fluidized bed of nanocomposite material (Nafion mass fraction is 13%);

[0042] 3) Carry out adsorption filtration and ultrafiltration membrane filtration;

[0043] 4) Under normal pressure at 100°C for 40 minutes;

[0044] 5) Under the conditions of 180°C and vacuum degree less than -0.099MPa, carry out decompression for 2 hours to obtain hydroxyl silicone oil. The solvent and unreacted low molecular weight compounds in the reaction system enter the reaction system for recycling after detecting the content of each component .

Embodiment 2

[0046] 1) Add hexamethylcyclotrisiloxane, acetone and deionized into the mixing tank according to the molar ratio of 1:4:1.2, and stir and mix for 20 minutes;

[0047] 2) Transfer the material into a Nafion / SiO 2 Catalytic reaction at 50°C for 50 minutes in a fluidized bed of nanocomposite material (Nafion mass fraction is 20%);

[0048] 3) Carry out adsorption filtration and ultrafiltration membrane filtration;

[0049] 4) Under normal pressure at 80°C for 60 minutes;

[0050] 5) Under the conditions of 150°C and vacuum less than -0.099MPa, carry out decompression for 3 hours to obtain hydroxyl silicone oil. The solvent and unreacted low-molecular compounds in the reaction system enter the reaction system for recycling after detecting the content of each component .

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Abstract

The invention discloses hydroxyl silicone oil and a continuous preparation method thereof.The method includes the following steps of firstly, adding hexamethyl cyclotrisiloxane, solvent and water into a mixing kettle to be evenly stirred and mixed, and transferring the mixture into a sulfuration bed filled with a catalyst to sufficiently react; secondly, conducting adsorption filtering, ultrafiltration membrane filtering, normal-pressure devolatiligation and reduced-pressure devolatiligation to obtain the hydroxyl silicone oil, recovering solvent and unreacted low-molecular compounds, detecting the contents of all components and then conducting recycling.The method is high in efficiency, low in energy consumption, free of pollutant emission, clean, sanitary and low in production cost, solvent and unreacted low-molecular compounds used in reaction can enter a reaction system to be recycled after the contents of all the components are detected, and the method is free of pollutant emission, green and environmentally friendly.The hydroxyl silicone oil is low in viscosity, high in product purity, low in annulus content, low in impurity ion content and high in storage stability.

Description

technical field [0001] The invention relates to a hydroxyl silicone oil and a continuous preparation method thereof. Background technique [0002] In the industry, fumed silica is generally used to reinforce thermally vulcanized silicone rubber, because the active Si-OH contained on the surface of fumed silica will interact with the Si-O bond or terminal Si-OH in the raw silicone rubber molecule to generate hydrogen bond or condensation, which makes it difficult for silica to disperse evenly in the silicone rubber compound, and the mixed compound will gradually harden during storage, reducing plasticity, making it impossible to rework, reducing processing performance, and resulting in " structuring” phenomenon. In order to improve the affinity between silicone rubber particles and filler particles, reduce the formation of hydrogen bonds, improve the dispersion of fillers in the rubber compound, improve the mixing process and storage stability, prevent and weaken this contin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/16C08G77/08C08G77/06
CPCC08G77/06C08G77/08C08G77/16Y02P20/10
Inventor 王跃林谌绍林冯钦邦吴利民
Owner GUANGZHOU DAOLIN SYNTHETIC MATERIALS CO LTD
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