Stable methylacryloyl cage type silsesquioxane emulsion with Pickering effect and preparation thereof

A technology of methacryloyloxy cage and silsesquioxane, which is applied in the field of emulsion polymerization preparation, can solve the problems of narrow range of inorganic particles, and achieve the effects of simple post-processing, stable emulsion, and reduced use

Active Publication Date: 2014-07-16
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even so, the range of inorganic particles involved in Pickering emulsions is still relatively narrow
However, MA-POSS has an organic-inorganic

Method used

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  • Stable methylacryloyl cage type silsesquioxane emulsion with Pickering effect and preparation thereof
  • Stable methylacryloyl cage type silsesquioxane emulsion with Pickering effect and preparation thereof
  • Stable methylacryloyl cage type silsesquioxane emulsion with Pickering effect and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1: Preparation of MA-POSS Stabilized Emulsion with Pickering Effect

[0039] (1) Preparation of pre-emulsion

[0040] Add 10 g of styrene to the four-necked flask, T 8 -MA-POSS1g, water 20g, sodium dodecyl sulfonate 0.037g, OP-100.018g, 3g sodium bicarbonate solution with mass concentration of 3% to adjust the pH to 7~8. A mechanical stirrer was used to carry out the stirring reaction, the rotating speed was 700 rpm, and the pre-emulsification was stopped after 40 min at normal temperature to obtain a white emulsion.

[0041] (2) Preparation of polymer emulsion by seed emulsion polymerization

[0042] The pre-emulsion obtained in the above steps was transferred to a constant pressure funnel, and about 20% of the remaining in the flask was used as a seed, and an initiator solution, that is, 3 g of a 3% ammonium persulfate (APS) solution, was added, and about 20% of the ammonium persulfate (APS) solution was added to the flask. APS solution. A constant pressur...

Embodiment 2

[0045] Example 2: Preparation of MA-POSS Stabilized Emulsion with Pickering Effect

[0046] (1) Preparation of pre-emulsion

[0047] Add 10 g of styrene to the four-necked flask, T 8 -MA-POSS 2g, water 20g, sodium dodecyl sulfonate 0.028g, OP-100.014g, 4g sodium bicarbonate solution with a mass concentration of 3% to adjust the pH to 7-8. The stirring reaction was carried out with a mechanical stirrer, the rotating speed was 700 rpm, and the temperature was normal. After 40 min, the pre-emulsification was stopped to obtain a white emulsion.

[0048] (2) Preparation of polymer emulsion by seed emulsion polymerization

[0049] The pre-emulsion obtained in the above steps was transferred to a constant pressure funnel, and the remaining about 20% in the flask was used as a seed. A constant pressure funnel was loaded on the four-necked flask, and the pre-emulsion was uniformly added dropwise, and the constant-flow pump was uniformly added dropwise to the ammonium persulfate sol...

Embodiment 3

[0052] Example 3: Preparation of MA-POSS Stabilized Emulsion with Pickering Effect

[0053] (1) Preparation of pre-emulsion

[0054] Add 10 g of styrene to the four-necked flask, T 8 -MA-POSS 3g, water 22g, sodium dodecyl sulfonate 0.017g, OP-100.009g, 4g sodium bicarbonate with a mass concentration of 4% to adjust the pH to 8-9. A mechanical stirrer was used to carry out the stirring reaction, the rotating speed was 700 rpm, and the pre-emulsification was stopped after 40 min at normal temperature to obtain a white emulsion.

[0055] (2) Preparation of polymer emulsion by seed emulsion polymerization

[0056] The pre-emulsion obtained in the above steps was transferred to a constant pressure funnel, and about 30% of the remaining in the flask was used as a seed. A constant pressure funnel was loaded on the four-necked flask, and the pre-emulsion was uniformly added dropwise, and the constant-flow pump was uniformly added dropwise to the ammonium persulfate solution, the re...

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Abstract

The invention belongs to the technical field of emulsion polymerization preparation, and discloses a stable methylacryloyl cage type silsesquioxane emulsion with a Pickering effect and a preparation method thereof. The preparation method comprises the steps: making methylacryloyl cage type silsesquioxane and a polymerization monomer carry out an emulsion reaction in a water system under the action of an emulsifying agent to prepare a pre-emulsion, and then by adopting a seed emulsion polymerization method, performing a polymerization reaction under the action of an initiating agent to obtain the emulsion with the Pickering effect. According to the preparation method, an MA-POSS (methyl methacrylate polyhedral oligomeric silsesquioxane) is polymerized with St (styrene), MMA (Methyl Methacrylate) or BA (butyl acrylate) instead of a conventional emulsifying agent to obtain the emulsion with the Pickering effect, because the MA-POSS has an organic-inorganic nano hybridization structure, and is larger in molecular weight, favorable heat performance, mechanical performance and the like of the MA-POSS are introduced into the polymer emulsion, the performances such as heat resistance and stretching of the polymer can be effectively improved, and the application range of the Pickering emulsion is greatly enlarged.

Description

technical field [0001] The invention belongs to the technical field of emulsion polymerization preparation, in particular to a methacryloxy clathrate silsesquioxane (MA-POSS)-stabilized emulsion with Pickering effect and a preparation method thereof. Background technique [0002] Cage silsesquioxane (POSS), also known as polyhedral cage silsesquioxane, is a general term for a class of silsesquioxanes with a lantern-like structure. In a broad sense, in addition to complete cage silsesquioxanes, it also includes partial open cage silsesquioxanes. According to the number of silicon atoms in POSS, they are also referred to as T for short. 8 -POSS([RSiO 1.5 ] 8 ), T 10 -POSS([RSiO 1.5 ] 10 ) and T 12 -POSS([RSiO 1.5 ] 12 ). In previous applications, POSS was mostly physically doped in polymers to improve the thermal stability and mechanical properties of polymers, reduce the dielectric constant, or chemically bonded by chemical end-capping, suspension connection or cros...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F220/14C08F220/18C08F230/08C08F2/26C08F2/30
Inventor 许凯邢玉秀彭军林伟鸿陈鸣才
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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