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A kind of hydroxy silicone oil and its continuous preparation method

A technology of hydroxysilicone oil and hexamethylcyclotrisiloxane is applied in the field of hydroxysilicone oil and its continuous preparation, which can solve the problems of low catalytic efficiency, small effective surface area, low conversion rate, etc. Large contact area and good storage stability

Active Publication Date: 2018-08-21
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 hydroxysilicone oil. The method uses perfluorosulfonic acid ion exchange resin (Nafion resin) as a catalyst to prepare low-viscosity hydroxysilicone oil. Although perfluorosulfonic acid resin is acidic and Concentration 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

Method used

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  • A kind of hydroxy silicone oil and its continuous preparation method
  • A kind of hydroxy silicone oil and its continuous preparation method

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preparation example Construction

[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, and 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, step 1) described catalyst is Nafion / SiO 2 The nanocomposite material, wherein the mass fraction of Nafion is 5-40%.

[0032] Further preferably, the Naf...

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 the Nafion / SiO 2 In the fluidized bed of the nanocomposite material (the mass fraction of Nafion is 13%), catalyzed reaction 40min under 60 ℃;

[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 less than -0.099MPa, carry out decompression for 2 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 .

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 the Nafion / SiO 2 In the fluidized bed of the nanocomposite material (the mass fraction of Nafion is 20%), the catalytic reaction was carried out at 50° C. for 50 minutes;

[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

Disclosed in the present invention are a hydroxyl silicone oil and a continuous method for preparing same. The continuous method for preparing the hydroxyl silicone oil includes following steps of: 1) adding hexamethyl cyclotrisiloxane, a solvent and water into a mixing kettle, stirring and mixing them evenly, and then transferring the mixture into a fluidized bed filled with a catalyst to react sufficiently; 2) carrying out an adsorption filtration and an ultrafiltration membrane filtration, removing low molecular weight compounds at normal pressure and removing low molecular weight compounds at a reduced pressure so as to obtain the hydroxyl silicone oil, recovering the solvent and unreacted low molecular weight compounds, detecting the content of each component and then recycling them. The method of the present invention has high efficiency and low energy consumption, being free of pollutant emission, being clean and environmentally friendly, and having low production cost. The solvent used in the reaction and the unreacted low molecular weight compounds can be entered into a reaction system to be recycled after the content of each component is detected, such that the method is free of pollutant emission, being green and environmentally friendly. The hydroxyl silicone oil of the present invention has low viscosity, high product purity, low content of rings, low content of impurities and high 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 Patents(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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