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Method for in-situ preparing nano-silicon dioxide/hydroxy terminated polydimethylsiloxane hybrid material

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

Active Publication Date: 2017-06-13
河南海博瑞硅材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Method for in-situ preparing nano-silicon dioxide/hydroxy terminated polydimethylsiloxane hybrid material
  • Method for in-situ preparing nano-silicon dioxide/hydroxy terminated polydimethylsiloxane hybrid material
  • Method for in-situ preparing nano-silicon dioxide/hydroxy terminated polydimethylsiloxane hybrid material

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Embodiment 1

[0027] A method for in-situ preparation of nano-silica / hydroxy-terminated polydimethylsiloxane hybrid material includes the following steps: DMC and tetramethylammonium hydroxide are added to a three-necked flask equipped with a reflux condenser, and Under stirring, the temperature was raised to 100°C and stirred at constant temperature for 50 min to make DMC ring open and pre-polymerization reaction occurred; then nano-silica was added and stirred at 100°C for 60 min without fractions distilled out; and the vacuum degree was -0.02 MPa Under the condition of ~-0.04 MPa, stir at a constant temperature of 100°C until no fractions are distilled out; cool to room temperature to obtain; wherein the mass ratio of DMC ring body, tetramethylammonium hydroxide and nano silica is 100: 2× 10 -4 :2.

Embodiment 2

[0029] A method for in-situ preparation of nano-silica / hydroxy-terminated polydimethylsiloxane hybrid material includes the following steps: DMC and tetramethylammonium hydroxide are added to a three-necked flask equipped with a reflux condenser, and Under stirring, the temperature was raised to 105℃, and stirred at constant temperature for 50 min to make DMC ring open and prepolymerization reaction occurred; then nano silica was added and stirred at 100℃ constant temperature for 60 min, and no fractions were distilled out; and the vacuum degree was -0.02 MPa Under the condition of ~-0.04 MPa, stir at 105℃ until no fractions are distilled out; cool to room temperature to get it; among them, the mass ratio of DMC monomer, tetramethylammonium hydroxide and nano silica is 100: 2× 10 -4 : 4.

Embodiment 3

[0031] A method for in-situ preparation of nano-silica / hydroxy-terminated polydimethylsiloxane hybrid material includes the following steps: DMC and tetramethylammonium hydroxide are added to a three-necked flask equipped with a reflux condenser, and Under stirring, the temperature was raised to 100°C and stirred at constant temperature for 50 min to make DMC ring open and pre-polymerization reaction occurred; then nano-silica was added and stirred at 100°C for 60 min without fractions distilled out; and the vacuum degree was -0.02 MPa Under the condition of ~-0.04 MPa, stir at a constant temperature of 100°C until no fractions are distilled out; cool to room temperature to obtain; wherein the mass ratio of DMC ring body, tetramethylammonium hydroxide and nano silica 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, and specifically relates to a method for preparing nano-silica / hydroxy-terminated polydimethylsiloxane hybrid materials in situ. Background technique [0002] Organic-inorganic hybrid materials are the fourth generation of new materials after single-component materials, composite materials and functionally graded materials. Among them, organic and inorganic components are combined by chemical bonds in a cross-linked network structure, and have both organic and inorganic materials. The performance advantages of objects have received widespread attention. [0003] Compared with other organic polymers, hydroxy-terminated polydimethylsiloxane (PDMS) has many unique features, such as electrical insulation, weathering resistance, ozone resistance, and physiological inertness. It is mainly used in silicone rubber In the base polymer. However, due to the small intermolecular forces of hydroxy-te...

Claims

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Application Information

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Patent Type & Authority Applications(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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