Preparation method of high molecular weight branched polymers

A branched polymer, high molecular weight technology, applied in the field of preparation of high molecular weight branched polymers, can solve the problems of limited types of thiol monomers, limited molecular weight of polymers, easy cross-linking of polymers, etc., and achieves a controllable structure. , The effect of simple components and high yield

Inactive Publication Date: 2019-11-26
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the amino or mercapto monomers required for the preparation of branched polymers by the above method are toxic and unpleasant
In addition, the types of mercapto monomers are limited and unstable, and their polymerization systems are prone to crosslinking
[0003] Although the basic catalyst (K 2 CO 3 , NaH, Potassium tert-butoxide, etc.) can also prepare branched polymers with Michael addition polymerization, but the reaction conditions required for the polymers prepared by them are relatively harsh, and the molecular weight of the polymers obtained is also limited, and the polymer used for polymerization The monomers are all ABs that require multi-step tedious synthesis 2 monomer

Method used

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  • Preparation method of high molecular weight branched polymers
  • Preparation method of high molecular weight branched polymers
  • Preparation method of high molecular weight branched polymers

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Experimental program
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Effect test

Embodiment 1

[0025] Trimethylolpropane (0.134 g, 1 mmol) and 1,6-hexanediol diacrylate (0.226 g, 1 mmol) dissolved in DMF (1.217 g) were added to a dehydrated and argon-purged polymerization bottle , after freezing and evacuating argon for three times, under the protection of argon, use a 100 μL micro-injector to add the catalyst t-BuP at a rate of 3-5 s per drop 2 (50 μL, 0.1 mmol) was reacted at 25° C. for 60 min. After the reaction was completed, acetic acid was added to terminate the reaction, diluted with dichloromethane, and settled in n-hexane through an acidic alumina column to obtain a hydroxyl-terminated polymer with a yield of 52.5%. Adopt nuclear magnetic resonance spectrometer and gel permeation chromatography to analyze polymer, the result is as follows: Gel permeation chromatography relative weight-average molecular weight M w.GPC =6461g / mol, molecular weight distribution PDI=1.90, absolute weight average molecular weight M w.MALLS =33080g / mol, the branching degree DB calc...

Embodiment 2

[0027] Trimethylolpropane (0.134 g, 1 mmol) and 1,6-hexanediol diacrylate (0.226 g, 1.5 mmol) dissolved in DMF (1.217 g) were added to a dehydrated and argon-purged polymerization bottle In the process, after freezing and evacuating argon for three times, under the protection of argon, add the catalyst t-BuP with a 100 μL micro-injector at a rate of 3-5 s per drop. 2 (50 μL, 0.1 mmol) was reacted at 25° C. for 60 min. After the reaction was completed, acetic acid was added to terminate the reaction, dichloromethane was diluted, and the acidic alumina column was settled in n-hexane to obtain a polymer containing hydroxyl groups and double bond ends with a yield of 58.6%. Adopt nuclear magnetic resonance spectrometer and gel permeation chromatography to analyze polymer, the result is as follows: Gel permeation chromatography relative weight-average molecular weight M w.GPC =7002g / mol, molecular weight distribution PDI=2.59, absolute weight average molecular weight M w.MALLS =5...

Embodiment 3

[0029] Trimethylolpropane (0.134 g, 1 mmol) and 1,6-hexanediol diacrylate (0.452 g, 2 mmol) dissolved in DMF (1.172 g) were added to a dehydrated and argon-purged polymerization bottle , after freezing and evacuating argon for three times, under the protection of argon, use a 100 μL micro-injector to add the catalyst t-BuP at a rate of 3-5 s per drop 2 (25 μL, 0.05 mmol) was reacted at 25° C. for 60 min. After the reaction was completed, acetic acid was added to terminate the reaction, diluted with dichloromethane, and settled in n-hexane through an acidic alumina column to obtain a double-bond-terminated polymer with a yield of 45.8%. Polymer is analyzed by proton nuclear magnetic resonance spectrometer and gel permeation chromatography, and the results are as follows: Gel permeation chromatography relative weight average molecular weight M w.GPC =4468g / mol, molecular weight distribution PDI=2.30, absolute weight average molecular weight M w.MALLS =21960g / mol, the branching...

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Abstract

Belonging to the field of polymer synthesis, the invention relates to a preparation method of high molecular weight branched polymers. The method includes: taking an alcoholic hydroxyl monomer as a hydroxyl monomer, adopting acrylic ester as a double-bond monomer, catalyzing the Oxa-Michael addition polymerization of hydroxyl and unsaturated double or triple bond in an organic solvent by organophosphorus nitrile base t-BuP2, thus preparing high molecular weight branched polymers with different terminal groups. The branched polymers prepared by the method provided by the invention have the characteristics of controllable and modifiable structure, and are suitable for application in different fields. The method has the advantages of mild reaction conditions, fast reaction, high efficiency and high yield, and the required monomers are all commercial monomers, the catalyst is free of metal residue, safe and environment-friendly, therefore the high molecular weight branched polymers can beused for large-scale production and application, and have huge application prospects.

Description

technical field [0001] The invention belongs to the field of high molecular synthesis, in particular to a preparation method of high molecular weight branched polymer. Background technique [0002] Branched polymers have a unique three-dimensional network structure, so they have the advantages of low viscosity, good solubility, and more functional end groups, and have been widely used in the fields of catalysis, coatings, adhesives, and nano-medicines. At present, various strategies are used to prepare branched polymers, such as atom transfer polymerization, ring-opening polymerization, free radical polymerization, condensation polymerization and other methods. Among them, Michael addition polymerization is based on the reaction of protons and unsaturated double bonds. It has the advantages of mild reaction conditions, high yield and simple post-treatment. It is also an effective method for preparing branched polymers. At present, more researches are based on Michael additi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/34
CPCC08G65/34
Inventor 蒋其民杨宏军黄文艳薛小强江力蒋必彪
Owner CHANGZHOU UNIV
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