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Preparation method of cagelike silsesquioxane-contained polymethyl methacrylate hybrid material

The technology of siloxane polymethyl methacrylate and methyl methacrylate is applied in the field of polymethyl methacrylate hybrid materials, and can solve the problem that the preparation process of polymethyl methacrylate/POSS hybrid materials is complicated, ATRP initiator POSS has long synthetic route and difficult to control reaction process, etc., to achieve the effect of short reaction route, simple synthesis conditions and simplified preparation process.

Inactive Publication Date: 2010-11-03
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the above-mentioned preparation method, the synthesis route of the ATRP initiator POSS used is relatively long, and the reaction process is difficult to control, resulting in a complicated preparation process of polymethyl methacrylate / POSS hybrid material, which is not conducive to future industrial applications.

Method used

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  • Preparation method of cagelike silsesquioxane-contained polymethyl methacrylate hybrid material
  • Preparation method of cagelike silsesquioxane-contained polymethyl methacrylate hybrid material
  • Preparation method of cagelike silsesquioxane-contained polymethyl methacrylate hybrid material

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preparation example Construction

[0016] The preparation method of polymethyl methacrylate hybrid material containing clathrate silsesquioxane of the present invention is realized by atom transfer radical polymerization, comprising the following steps:

[0017] The first step: Add initiator, catalyst and complexing agent in the dry reaction bottle, vacuumize, and fill with argon to react, wherein the initiator is octa(γ-chloropropyl)silsesquioxane, and the catalyst is chlorine Cuprous chloride or cuprous bromide, the complexing agent is 2,2'-bipyridine; the mass ratio of initiator to catalyst is 1.85:1~2.0:1, and the mass ratio of complexing agent to catalyst is 3.70:1~4.0 : 1. The ratio of the amount of methyl methacrylate monomer to the amount of the initiator is 750:1-900:1.

[0018] Step 2: Add solvent and methyl methacrylate monomer MMA, stir evenly, after heating the reaction, stop the reaction by freezing, such as about minus 18 degrees; the heating temperature is 80-100°C, and the reaction time is 5-2...

Embodiment 1

[0021] In a dry reaction flask, under the protection of argon, add 0.240 g of complexing agent 2,2′-bipyridine, 0.125 g of initiator octa(γ-chloropropyl) silsesquioxane, catalyst cuprous chloride 0.064g, vacuumize, fill with argon, repeat three times; inject 10mL toluene solvent and 10mL methyl methacrylate monomer, and react at 90°C for 15 hours. After the reaction, take out the reaction bottle and place it in the refrigerator to freeze to terminate the reaction. 5 mL of tetrahydrofuran was added to dissolve the polymer, filtered, and the filtrate was added to a large amount of methanol for precipitation. The precipitate was dissolved in tetrahydrofuran again, reprecipitated, and finally vacuum-dried to obtain the product with a yield of 17%.

[0022] In this embodiment, the polymethyl methacrylate hybrid material can be obtained by using toluene as a solvent. The number average molecular weight of the hybrid material is 102572g / mol, the molecular weight distribution index (P...

Embodiment 2

[0024] In a dry reaction flask, under the protection of argon, add 0.240 g of complexing agent 2,2′-bipyridine, 0.125 g of initiator octa(γ-chloropropyl) silsesquioxane, catalyst cuprous chloride 0.064g, vacuumize, fill with argon, repeat three times; inject 10mL isopropanol solvent and 10mL methyl methacrylate monomer, react at 80°C for 15 hours, after the reaction, take out the reaction bottle, put it in the refrigerator to stop To react, add 5 mL of tetrahydrofuran to dissolve the polymer, filter, add the filtrate to a large amount of methanol for precipitation, and dissolve the precipitate with tetrahydrofuran again, reprecipitate, and finally vacuum dry to obtain the product with a yield of 21%.

[0025] In this embodiment, the polymethyl methacrylate hybrid material can also be obtained by using isopropanol as a solvent. The number average molecular weight of the hybrid material is 28308g / mol, the molecular weight distribution index (PDI) is 1.25, and the glass transitio...

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Abstract

The invention discloses a preparation method of a cagelike silsesquioxane-contained polymethyl methacrylate hybrid material, which is realized through atom transfer radical polymerization (ATRP) and carried out according to the following steps of: adding an initiator, a catalyst and a complexing agent into a dry reaction bottle, evacuating, and filling argon for reaction; adding a solvent and a methyl methacrylate (MMA) monomer, uniformly stirring, heating for reaction, and then cooling to stop the reaction; adding a polymer generated by dissolving tetrahydrofuran into the reaction bottle, filtering, adding a filtrate into a methanol solution for precipitation to obtain a product, dissolving a precipitate through the tetrahydrofuran again, filtering, and then precipitating in the methanol solution again; and adding the precipitate into a vacuum drying box for drying. A POSS (Polyhedral Oligomeric Silsesquioxane) initiator used by the invention has simple synthesis condition, easy obtainment and shorter reaction route, and the preparation flow of the hybrid material is greatly simplified; the POSS-contained polymethyl methacrylate hybrid material has higher glass transition temperature (Tg), and the application field of polymethyl methacrylate is widened.

Description

technical field [0001] The invention belongs to the preparation technology of polymer-based organic-inorganic hybrid materials, in particular to a method for preparing polymethyl methacrylate hybrid materials containing clathrate silsesquioxane by means of atom transfer radical polymerization. Background technique [0002] Polymethyl methacrylate (PMMA for short) is a polymer with excellent transparency, weather resistance and ease of processing, but due to its inherent low glass transition temperature (T g ) and poor thermal stability, which limit its further application in many high-tech fields. [0003] Cage silsesquioxane (referred to as POSS) is a new type of nanomaterial that has emerged in recent years, and its molecular formula can be expressed as (RSiO 1.5 )n (n can generally be 6, 8, 10, etc.), which is composed of a rigid, structurally determined nanoscale inorganic core composed of silicon and oxygen and an organic-inorganic shell composed of an organic group R ...

Claims

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Application Information

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IPC IPC(8): C08F220/14
Inventor 汪信赵春宝张楠楠杨勇杨绪杰陆路德刘孝恒郝青丽
Owner NANJING UNIV OF SCI & TECH
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