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A kind of polyalkene with high 1,2-regioselectivity and its preparation method

A regioselective, polyalkene technology applied in the field of polymer materials

Active Publication Date: 2020-09-22
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the technical problem that existing polyalkenes do not have high 1,2-regioselectivity, the present invention provides a polyalkene with high 1,2-regioselectivity and a preparation method thereof

Method used

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  • A kind of polyalkene with high 1,2-regioselectivity and its preparation method
  • A kind of polyalkene with high 1,2-regioselectivity and its preparation method
  • A kind of polyalkene with high 1,2-regioselectivity and its preparation method

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preparation example Construction

[0065] Preparation of rare earth catalyst composition:

[0066] Preparation of Rare Earth Catalyst Composition 1: Add 10 μmol of the rare earth complex shown in formula 1, 10 μmol of [Ph 3 C][B(C 6 f 5 ) 4 ], 100 μmol triisobutylaluminum and toluene solvent, the concentration of the rare earth complex in the rare earth catalyst composition is 2.0mmol L –1 , and reacted for 2 minutes to obtain rare earth catalyst composition 1.

[0067] Preparation of rare earth catalyst composition 2: at 25°C, add 10 μmol of the rare earth complex shown in formula 2, 10 μmol of [Ph 3 C][B(C 6 f 5 ) 4 ], 100 μmol triisobutylaluminum and toluene solvent, the concentration of the rare earth complex in the rare earth catalyst composition is 2.0mmol L –1 , and reacted for 2 minutes to obtain rare earth catalyst composition 2.

[0068] Preparation of rare earth catalyst composition 3: at 25°C, add 10 μmol of the rare earth complex shown in formula 3, 10 μmol of [Ph 3 C][B(C 6 f 5 ) 4 ],...

Embodiment 1

[0126] Take 1ml of the toluene solution of catalyst combination 1, put it in a polymerization bottle treated with anhydrous and oxygen-free treatment, add 5.0mmol of allene monomer A, carry out the polymerization reaction at -40°C for 36 hours, add 2ml with a volume concentration of 10% The ethanol solution of hydrochloric acid terminates the polymerization reaction, and the reaction solution is poured into 100ml of methanol for sedimentation to obtain polydecyl allene with 1,2-regioselectivity>99%; then the obtained polymer is placed in a vacuum drying oven for 48 After 1 hour, a high 1,2-regioselective polydecyl allene with a constant dry weight was obtained, with a net weight of 0.905 g. Overall conversion 100%. With NMR spectrum ( 1 H NMR) and carbon nuclear magnetic spectrum ( 13 CNMR) analysis obtains the 1,2-regioselectivity >99% of highly 1,2-regioselective polydecyl allene, as Figure 7 and Figure 8 Shown; GPC analysis obtains > 99% average molecular weight (M n...

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Abstract

The invention discloses polyallene with high 1,2-regioselectivity and a preparation method thereof and belongs to the technical field of high molecular polymers. The structure of the polyallene with high 1,2-regioselectivity is shown as a general formula (I); the polyallene with high 1,2-regioselectivity, provided by the invention also has the following characteristics that the number average molecular weight is 0.1*10<4> to 300*10<4> and the ratio of repeating unit numbers n and m in the polymer is not lower than 9: 1. According to the polyallene with high 1,2-regioselectivity, provided by the invention, a terminal double bond is introduced and can be used as a precursor of a functional polymer, and the polyallene is a brand new high molecular polymer; a catalyst combination used by the preparation method of the polyallene with high 1,2-regioselectivity, provided by the invention, comprises a rare earth compound, an alkyl aluminum compound and organic boron salt; and the polyallene with high 1,2-regioselectivity is synthesized by utilizing a coordination polymerization method for the first time and the method has very good innovativeness.

Description

technical field [0001] The invention relates to a novel polymer, in particular to a polyalkene with terminal double bond and high 1,2-regioselectivity and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] The polymerization of allenes was first achieved by Baker in 1963 by catalyzed polymerization using transition metal catalysts. Polyalkenes are very attractive precursors for post-functionalization due to their unreacted double bonds. The polyalkene obtained by high 1,2-regioselective polymerization has high application value due to the special reactivity of the terminal double bond. However, it is difficult to achieve high 1,2-regioselective polymerization of allene with substituents. . Therefore, selecting suitable catalytic conditions to achieve high 1,2-regioselective polymerization of allene monomers has been a subject that many scientific and technological workers are committed to solving. In 1997, a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F236/20C08F4/52C08F4/54C08F8/06C08F8/42
CPCC08F8/06C08F8/42C08F236/20C08F4/52C08F4/545
Inventor 崔冬梅钟元昊吴春姬
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI