Polymethano-poly(methyl)acrylic ester two-block copolymer and preparation method thereof

A technology of block copolymers and acrylates, which is applied in the field of polymethylene/polyacrylate diblock copolymers and its preparation, can solve the problems of preparing macromolecular initiators, block copolymer research and Application and other issues

Inactive Publication Date: 2009-06-17
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although they and other research groups have done some group conversion work [US5476915; Macromolecules 2000, 33, 4295], they have not used it to perform group conversion to prepare macromolecular initiators, nor have they prepared polymethylene-based Research and Application of Block Copolymer

Method used

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  • Polymethano-poly(methyl)acrylic ester two-block copolymer and preparation method thereof
  • Polymethano-poly(methyl)acrylic ester two-block copolymer and preparation method thereof
  • Polymethano-poly(methyl)acrylic ester two-block copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 32

[0040] The specimens in Example 32 were prepared using a micro-injection molding machine (ISO527-2-A5a tensile test mold).

[0041] The bromine content of the polymer is based on 1 H-NMR spectrum calculated.

Embodiment 1

[0043] The preparation of polymethylene / poly(meth)acrylate block copolymer with controllable structure of the present invention:

[0044] In a dry 10mL round bottom flask A with a magnetic stirrer, add 0.10g (0.054 mmol Br) of macromolecular initiator MI-01 (M n = 1856, PDI = 1.23, n = 120, bromine content = 540 μmol / g polymer, 1 H NMR (500MHz, δ ppm): 3.92(t, 2H), 1.69(s, 6H), 1.42(t, 2H), 1.10(m, 240H), 0.67(s, 12H), ), after 30min of vacuum , filled with nitrogen. In another 10mL dry round-bottomed flask B with a magnetic stir bar, add CuBr 7.7mg (0.054mmol), PMDETA (N,N,N',N',N"-pentamethyldi Ethylene triamine) 22.5 L 0.108mmol), MMA (methyl methacrylate) 0.58mL (5.4mmol, after vacuum distillation) and toluene 2.5mL (after metal sodium reflux treatment), after stirring for 30min, under nitrogen protection The above mixture was transferred to the round bottom flask A with a dry double-ended needle tube, and the polymerization reaction was carried out at 90 ° C for 6 h. A...

Embodiment 2～ Embodiment 7

[0046] The preparation of polymethylene / poly(meth)acrylate diblock copolymer with controllable structure of the present invention:

[0047] Operation is basically the same as embodiment 1. The difference is that in the ATRP polymerization reaction, the types and amounts of catalysts and ligands, reaction solvents and amounts thereof, reaction temperature and reaction time are not completely the same as in Example 1. Structure-controllable polymethylene / poly(meth)acrylate diblock copolymers P-02 (n=120, m=20), P-03 (n=120, m=24), P-03 (n=120, m=24), P-04(n=120, m=50), P-05(n=120, m=92), P-06(n=120, m=66) and P-07(n=120, m=96 ).

[0048] The specific experimental conditions and polymer characterization data are shown in Table 1:

[0049] In the products of Examples 2-7, R 1 and R 2 Both CH 3 .

[0050] Table 1

[0051]

[0052] Note: b-Py=2,2'-bipyridine or its alkyl derivatives, PMDETA (N,N,N',N',N"-pentamethyldivinyltriamine)

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Abstract

The invention discloses a structurally controllable polymethylene / poly(methyl)acrylic esters block copolymer and a preparation method thereof. The preparation method comprises the following steps: using a structurally controllable polymethylene macromolecule initiator having the number average molecular weight capable of being regulated in a certain range(500-1*10<5>g / mol) and the narrow molecular weight distribution (PDI is equal to 1.01-1.49) to initiate the atom radical transfer active free radical polymerization (ATRP) of a (methyl)acrylic esters polymerization monomer; and further preparing the polymethylene / poly(methyl)acrylic esters block copolymer (Mn is equal to *10<3>-1*10<6>g / mol, PDI is equal to1.01-1.50) which enables the molecular weight regulation for both blocks and has the narrow molecular weight distribution. The two-block copolymer can be applied to the blending study of polyolefin and the preparation of a polymer porous membrane as a compatilizer.

Description

technical field [0001] The invention relates to a structurally controllable polymethylene / poly(meth)acrylate diblock copolymer and a preparation method thereof, belonging to the technical field of polyolefin functionalization. Background technique [0002] Because of its good mechanical properties and chemical stability, low moisture absorption, easy processing, low price and recyclability, polyolefin has become one of the polymer materials with the largest amount and the widest application range. development plays a very important role. However, due to the non-polar molecular chain of polyolefin, the surface energy is very low, resulting in polyolefin adhesion, printing and dyeing, gas permeability, antistatic properties and compatibility with other polar polymer materials or inorganic fillers. Poor, resulting in its scope of application has been limited. Therefore, on the basis of maintaining the original excellent properties of polyolefins, introducing polar groups, rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00
Inventor 马志陈健壮李剑赵巧玲黄晋
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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