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Polyhedron oligomerization sesquialter siloxane-based segmented copolymer and preparation method thereof

A block copolymer, siloxane-based technology, applied in the field of copolymers, can solve the problem of phase separation structure loss of nano-hybrid materials and other problems

Inactive Publication Date: 2013-08-07
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, co-curing and end group chemical reactions are widely studied due to the variety of functional groups; and blending often causes the macroscopic phase separation structure to lose its characteristics of nano-hybrid materials.

Method used

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  • Polyhedron oligomerization sesquialter siloxane-based segmented copolymer and preparation method thereof
  • Polyhedron oligomerization sesquialter siloxane-based segmented copolymer and preparation method thereof
  • Polyhedron oligomerization sesquialter siloxane-based segmented copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Prepare MAiBuPOSS:CDB:AIBN=90:3:1 benzene solution system, the monomer concentration is 0.3mmol / ml, put it in a flask for freezing and degassing, and put it in an oil bath at 65°C for 24h, then freeze to stop the reaction. Add a small amount of tetrahydrofuran to dilute, then precipitate with methanol, and dissolve the precipitate repeatedly until the existence of POSS monomer is not detected by NMR. Vacuum drying obtains pink polymethacryloxypropyl POSS (MCTA1), which 1 HNMR picture as shown figure 1 shown. According to the molar ratio of ethyl acrylate (EA): polymethacryloxypropyl POSS (MCTA1): initiator (AIBN) = 1440: 3: 1, prepare a benzene solution. Sealed after argon replacement, 65 ° C oil bath for 24 hours, freezing to stop the reaction, adding a small amount of benzene to dilute and then precipitate with methanol, repeat 2 times, and dry to obtain polymethacryloxy isobutyl POSS-polyethylacrylate block copolymer BCP1, its 1 HNMR picture as shown figure 2 A...

Embodiment 2

[0027] Similar to Example 1, the difference is that the reaction time of step 2 is 48h, and all the other are the same as Example 1. Obtain polymethacryloxy isobutyl POSS-polyethylacrylate block copolymer BCP2, 1 The POSS content was determined to be 54.5% by HNMR.

Embodiment 3

[0029] Similar to Example 1, the difference is that the reaction time of step 1 is 4h, and CTA1 is obtained. All the other are with embodiment 1, obtain polymethacryloxy isobutyl group POSS-polyethylacrylate block copolymer BCP3, 1 The POSS content was determined to be 10% by HNMR.

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Abstract

The invention discloses polyhedron oligomerization sesquialter siloxane (POSS)-based segmented copolymer and a preparation method thereof, and relates to copolymer. Polymethyl methacryl oxygen propyl POSS is used as a first block, and poly(methyl)acrylate is used as a second block copolymer. The preparation method comprises the following steps of: putting the solution of a POSS monomer, a chain transfer agent and an initiator into a reaction vessel; freezing, degassing and then sealing; reacting; performing liquid nitrogen frozen, and stopping the reaction; adding tetrahydrofuran for dilution; precipitating by using methanol; repeatedly dissolving precipitates until the POSS monomer cannot be detected by nuclear magnetism; drying to obtain the pink polymethyl methacryl oxygen propyl POSS;adding the initiator, a second monomer and a solvent into the polymethyl methacryl oxygen propyl POSS; performing argon displacement, and then sealing; reacting; performing liquid nitrogen frozen, and stopping the reaction; adding benzene for dilution; precipitating by using the methanol; and drying to obtain the POSS-based segmented copolymer.

Description

technical field [0001] The invention relates to a copolymer, in particular to a polyhedral oligomerized silsesquioxane block copolymer and a preparation method. Background technique [0002] Polyhedral oligomeric silsesquioxanes (Polyhedral oligomeric silsesquioxanes, POSS) has a cage structure, and its classic structural formula is (RSiO 1.5 )n (n≥4, R=H, alkyl, aryl or organic functional group), between silicon dioxide (SiO 2 ) and silicone (R 2 Between SiO)n. POSS has a diameter of about 1.5-3nm and a molecular weight of up to 1000. It is considered to be "the finest form of silicon oxide that can exist", and is also considered to be a molecular sieve at the molecular level. In 1946, Scott (1, Scott D W. Thermal Rearrangement of Branchedchain Methylpolysiloxanes [J]. J Am Chem Soc, 1946, 68: 356) obtained polymethylsilsesquioxane (CH 3 SiO 1.5 )n, but the research and development of POSS is slow. Until the 1990s, the U.S. Air Force (Edwards Air Force Base, CA) was ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F130/08C08F120/18
Inventor 戴李宗邓远名杨仓杰陈江枫罗伟昂曾碧蓉许一婷
Owner XIAMEN UNIV