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A method for in-situ preparation of nano-silica/hydroxyl-terminated polydimethylsiloxane hybrid material

A technology of hydroxyl-terminated polydimethylsiloxane and nano-silicon dioxide is applied in the field of in-situ preparation of nano-silica/hydroxyl-terminated polydimethylsiloxane hybrid materials, which can solve the problems of agglomeration and polymer rheology. Poor, large specific surface area of ​​nano-silica, etc., to achieve the effect of reducing viscosity

Active Publication Date: 2019-05-17
河南海博瑞硅材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are the following problems: 1. Nano-silica has a large specific surface area and high activity. In the high-viscosity PDMS matrix, nano-silica is difficult to effectively disperse, and it is easy to cause agglomeration; The hydroxyl group further plays a role in increasing the viscosity of PDMS, resulting in poor rheological properties of the polymer and difficulties in processing

Method used

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  • A method for in-situ preparation of nano-silica/hydroxyl-terminated polydimethylsiloxane hybrid material
  • A method for in-situ preparation of nano-silica/hydroxyl-terminated polydimethylsiloxane hybrid material
  • A method for in-situ preparation of nano-silica/hydroxyl-terminated polydimethylsiloxane hybrid material

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Embodiment 1

[0027] A method for preparing nano-silica / hydroxyl-terminated polydimethylsiloxane hybrid materials in situ, comprising the following steps: adding DMC and tetramethylammonium hydroxide to a three-necked flask equipped with a reflux condensation device, Warm up to 100°C under stirring, and stir at constant temperature for 50 minutes to make DMC ring-open and prepolymerization; then add nano-silica, stir at 100°C for 60 minutes, no distillate; Under the condition of MPa~-0.04 MPa, stir at a constant temperature of 100°C until no fraction distills out; cool to room temperature to obtain it; wherein, the mass ratio of DMC ring body, tetramethylammonium hydroxide and nano silicon dioxide is 100:2 ×10 -4 :2.

Embodiment 2

[0029] A method for preparing nano-silica / hydroxyl-terminated polydimethylsiloxane hybrid materials in situ, comprising the following steps: adding DMC and tetramethylammonium hydroxide to a three-necked flask equipped with a reflux condensation device, Heat up to 105°C under stirring, and keep stirring at constant temperature for 50 minutes to make DMC ring-opening and prepolymerization; then add nano-silica, stir at 100°C for 60 minutes, no distillate; Under the condition of MPa~-0.04 MPa, stir at a constant temperature of 105°C until no fraction distills out; cool to room temperature, and obtain it; wherein, the mass ratio of DMC monomer, tetramethylammonium hydroxide and nano-silicon dioxide is 100:2 ×10 -4 :4.

Embodiment 3

[0031] A method for preparing nano-silica / hydroxyl-terminated polydimethylsiloxane hybrid materials in situ, comprising the following steps: adding DMC and tetramethylammonium hydroxide to a three-necked flask equipped with a reflux condensation device, Warm up to 100°C under stirring, and stir at constant temperature for 50 minutes to make DMC ring-open and prepolymerization; then add nano-silica, stir at 100°C for 60 minutes, no distillate; Under the condition of MPa~-0.04 MPa, stir at a constant temperature of 100°C until no fraction distills out; cool to room temperature to obtain it; wherein, the mass ratio of DMC ring body, tetramethylammonium hydroxide and nano silicon dioxide is 100:2 ×10 -4 :6.

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Abstract

The invention discloses a method for in-situ preparing a nano-silicon dioxide / hydroxy terminated polydimethylsiloxane hybrid material. The method comprises the following steps: heating cyclosiloxane and a catalyst to 95-105 DEG C under a stirring state, stirring for 30-120 minutes to open loop of cyclosiloxane and perform prepolymerization reaction; then, adding nano-silicon dioxide, and stirring at the constant temperature of 95-105 DEG C until no fraction is distilled out; and stirring under a condition that the vacuum degree is negative 0.02MPa-negative 0.09MPa until no fraction is distilled out, wherein the mass ratio of cyclosiloxane monomer to the catalyst to nano-silicon dioxide is 100:5*10<4>-2*10<4>:(2-18). According to the hybrid material prepared by the method, the rheological property of the hybrid material is improved, nano-silicon dioxide and PDMS are bonded through chemical bonds, and the bonding mode of inorganic filler and polymer matrix is changed.

Description

technical field [0001] The invention belongs to the technical field of nano-hybrid materials, in particular to a method for in-situ preparation of nano-silica / hydroxyl-terminated polydimethylsiloxane hybrid materials. Background technique [0002] Organic-inorganic hybrid materials are the fourth generation of new materials after single-component materials, composite materials and functionally graded materials, in which organic components and inorganic components are chemically bonded in a cross-linked network structure, combining organic and inorganic Because of its performance advantages, it has received extensive attention. [0003] Compared with other organic polymers, hydroxyl-terminated polydimethylsiloxane (PDMS) has many unique properties, such as electrical insulation, weathering resistance, ozone resistance, physiological inertness, etc. It is mainly used in the silicone rubber in the base polymer. However, due to the small intermolecular force of hydroxyl-termin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08G83/001
Inventor 张治军程煜李小红刘培松徐凯
Owner 河南海博瑞硅材料科技有限公司
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