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Polymethylene-based star polymer, preparation method and application of polymethylene-based star polymer

A star-shaped polymer, polymethylene technology, applied in the field of polyolefin functionalization, can solve the problem of not much research on synthesis and performance

Inactive Publication Date: 2012-08-15
SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Star polymers have good rheological properties, mechanical properties, etc. There are not many studies on the synthesis and performance of (Macromolecules 2010, 43, 8331; Macromolecules 2010, 43, 4889; Macromolecules 2009, 42, 2313)

Method used

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  • Polymethylene-based star polymer, preparation method and application of polymethylene-based star polymer
  • Polymethylene-based star polymer, preparation method and application of polymethylene-based star polymer
  • Polymethylene-based star polymer, preparation method and application of polymethylene-based star polymer

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Experimental program
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Embodiment 19

[0098] The specimens in Example 19 were prepared with a micro injection molding machine (ISO527-2-A5a tensile test mold). Scanning electron microscope pictures were observed and measured on a scanning electron microscope (JSM-6390LV). The infrared spectrograms of the samples in the examples were obtained by testing on Nicolet AVATAR-360 using potassium bromide pellets.

[0099] The bromine content of the polymer was tested by ion chromatography.

Embodiment 1

[0101] The preparation of star polymethylene of the present invention:

[0102] In a dry 150mL round bottom flask with a magnetic stir bar, add 0.50g (0.25mmol) PM under nitrogen protection 2K -OH (K=1000g / mol, the same below. 1 H NMR (500MHz, D 4 -o-dichlorobenzene, 80°C, δppm): 3.60 (t, 2H), 1.55 (t, 2H), 1.20-1.46 (m, 280H), 0.91-0.94 (m, 12H). m n =1800g / mol, PDI=1.09), after vacuuming for 10min, fill with nitrogen. Add 75mL of dry toluene (refluxing with sodium metal), stir at 90°C for 0.5h to dissolve completely, and quickly add 2.5mol / L n-butyllithium n-hexane solution (0.11mL, 0.27mmol) after cooling down to room temperature, and stir After 30min, a toluene solution of p-toluenesulfonyl chloride (0.60mmol, 0.114mg, 10mL) was added, and refluxed overnight. After the reaction, it was directly precipitated in methanol, and the filtered solid was dissolved in toluene and methanol precipitated twice to obtain 0.52g (97% )PM 2K -OTs.

[0103] 0.127g (1.95mmol) NaN 3 ...

Embodiment 2

[0110] The preparation of star polymethylene of the present invention:

[0111] In a dry 150mL round bottom flask with a magnetic stir bar, add the macroinitiator PM under nitrogen protection 2K COC(CH 3 ) 2 -Br 0.20g (0.11mmol Br, M n = 1860 g / mol, PDI = 1.23, bromine content = 0.54 μmol / g polymer. 1 H NMR (500MHz, δppm): 3.92(t, 2H), 1.69(s, 6H), 1.42(t, 2H), 1.10(m, 240H), 0.67(s, 12H)) and 0.072g (1.1mmol) NaN 3 , then add 50mL of toluene and 25mL of DMF, reflux for 24h, precipitate in a mixed solvent of methanol and water (90:10, v / v), filter and wash the filter cake with water and acetone three times, and vacuum dry at 50°C for 24h to obtain 0.18g (92% yield) PM 2K COC(CH 3 ) 2 -N 3 .

[0112] In another 10mL dry round bottom flask B with a magnetic stir bar, add 0.15g (0.108mmol) PM under nitrogen protection 2K COC(CH 3 ) 2 -N 3 , 7.7mg (0.054mmol) CuBr, 0.15g (0.108mmol) T' 2 , 22.5μL (0.108mmol) PMDETA (N, N, N', N', N"-pentamethyldivinyltriamine) and d...

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Abstract

The invention discloses a polymethylene-based star polymer. A synthetic method for the polymethylene-based star polymer includes: connecting polymethylene including a nitrine functional group at a chain end or a polymethylene-based block copolymer onto a central nucleus including alkynyl by means of click chemistry, so that the polymethylene-based star polymer is prepared finally. The number-average molecular weight (Mn) of polymethylene chain segments can be regulated within a certain range of 500-1X105g / mol, and the polymethylene chain segments have narrow molecular weight distribution (PDI=1.01-1.49). The polymethylene-based block copolymer is prepared by combining Ylide living polymerization with other living polymerization methods (atom group transfer living radical polymerization or ring-opening polymerization), molecular weight of each of two blocks can be regulated, and the two blocks have narrow molecular weight distribution (Mn=1X103-1X105g / mol, and PDI=1.01-1.50). The star polymer can serve as blended compatilizer excellent in performance to be used for preparing blend of polyolefin / other polymers, so as to be of great significance on expansion on functionalized polyolefin.

Description

technical field [0001] The invention relates to a polymethylene-based star polymer, a preparation method and an application thereof, and belongs to the technical field of polyolefin functionalization. Background technique [0002] Polyolefin is one of the polymer materials with the largest consumption and the widest range of applications. However, the polyolefin molecular chain is non-polar, which limits its application range. Therefore, designing polyolefins with special structures or introducing polar groups, reactive groups or other functional groups into polyolefin molecules to functionalize polyolefins is an important way to achieve high performance polyolefin materials[ Chung, T.C.Functionalization of Polyolefins, Academic Press, London, 2002; Prog.Polym.Sci.2002, 27, 1347; CN 156617A; ZL 03141200.9; Hu Y L, Qiao J L, Lu L X ). Functionalization and Modification of Polyolefins-Science and Technology. Beijing: Chemistry Industry Press, 2006.1-68]. After functionalize...

Claims

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Application Information

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IPC IPC(8): C08G81/00C08G81/02C08L87/00C08L53/00C08L23/00
Inventor 马志陈健壮赵巧玲黄晋
Owner SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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