Method for preparing three hetero arms asteroid polymer

A technology of star structure and polymer, which is applied in the field of preparation of three heteroarm star structure polymers, can solve problems such as difficulties and achieve good controllability and strong universal significance

Inactive Publication Date: 2008-03-19
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, although this method has certain advantages in operation, there are actually certain difficulties in the selection of small molecule "capping" reagents that meet this requirement.

Method used

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  • Method for preparing three hetero arms asteroid polymer
  • Method for preparing three hetero arms asteroid polymer
  • Method for preparing three hetero arms asteroid polymer

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0031]

[0032] 1. Preparation of block polymer polystyrene-b-polyethylene oxide (PS-b-PEO) containing protected hydroxyl groups in the middle of the chain segment

[0033] First, 3.91g (1.40 mmol, M n(SEC)=2,800g / mol) end group functionalized polystyrene macroinitiator in toluene to remove water azeotropically. Then dissolve it in 100mLTHF and add it into a 250mL dry and clean (baked under infrared lamp for 2h) ampoule bottle, and fill it with high-purity nitrogen to make the internal and external pressure of the ampoule bottle basically equal. Slowly add a THF solution of diphenylmethyl potassium (DPMK) dropwise with a disposable syringe until the system turns dark yellow. The ampoule was then placed in an ice-water bath, and 7.2 mL (6.26 g) of ethylene oxide (EO) was injected rapidly. Slowly raise the temperature to 50°C and continue the reaction for 96 hours. After the reaction, PS-b-PEO with a protected hydroxyl group in the middle of the block polymer chain segment ...

Embodiment 2

[0040]

[0041] 1.20g (0.17mmol, M n(NMR) =7,100g / mol) block polymer PS-b-PEO into a 50mL ampoule, then add (45mL) toluene to remove water azeotropically, extract the solvent under vacuum, seal the cork tightly, and freeze in a vacuum system— Pump-thaw cycle three times. Then add a certain amount of THF, DPMK (5mL) and 1-ethoxyethyl glycidol (EEGE, 0.9mL, 0.90g) sequentially with a disposable syringe, seal it and place it in an oil bath at 60°C for 48h. After cooling to room temperature, the crude product was dissolved in tetrahydrofuran, precipitated in petroleum ether (30-60° C.), and filtered. The obtained product was dried in a vacuum oven at 45° C. for 12 h to constant weight to obtain a triblock star heteroarm polymer star (PS-PEO-PEEGE).

Embodiment 3

[0043]

[0044] Identical to the removal process of the protective group in Example 1, the protective group on the PEEGE segment in the triblock star heteroarm polymer star (PS-PEO-PEEGE) in Example 2 is removed, and then Precipitate in petroleum ether (30-60°C), and dry in a vacuum oven at 45°C for 12h to constant weight to obtain a triblock star heteroarm polymer star (PS-PEO-PG).

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Abstract

The invention belonging to the technical field of polymer synthetic chemistry relates to a preparation method of an ABC miktoarm star-structured polymer. The Omega-end contains both protective hydroxyl and active hydroxyl or sulfhydryl compound as initiators, the active hydroxyl or the sulfhydryl are utilized to initiate a second monomer to carry out ring-opening polymerization, after being blocked, the polymerized active hydroxyl becomes inert group, and then the protected hydroxyl in the middle of a chain section is deprotected under the acidic environment. The hydroxyl is utilized to initiate a third monomer to carry out ring-opening polymerization, or after the hydroxyl is modified as a bromine atom, the third monomer is initiated to carry out atom transfer radical polymerization, or after the hydroxyl is modified as trithiocarbonate group, the third monomer is initiated to prepare the ABC miktoarm star-structured polymer by reversible addition fragmentation chain transfer (raft) polymerization. The invention can combine different polymerization mechanisms to broaden the types of ABC miktoarm star-structured polymer.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis chemistry, and in particular relates to a preparation method of a polymer with a three-arm star structure. technical background [0002] The three-heteroarm star-shaped polymer with regular structure has a microphase morphology different from that of ternary or binary block polymers due to its special structure. It has been predicted by computer simulation that star-shaped hetero-arm polymers have a variety of stable microphase morphologies, but in actual experimental studies, due to the deviation of the composition or structure of the synthesized star-shaped hetero-arm polymers from the ideal, or due to Due to the diversity of combinations of star-shaped hetero-arm polymers, it is often difficult to draw general conclusions about the microphase morphology of star-shaped hetero-arm polymers. As for the assembly behavior of star-shaped heteroarm structure polymers in solution, there are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F8/04C08F8/00
Inventor 黄骏廉王国伟罗晓兰
Owner FUDAN UNIV
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