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Method for preparing norbornene open-loop translocation polymer or addition polymer

A technology of norbornene and ring-opening metathesis, applied in the field of chemical industry

Inactive Publication Date: 2008-08-13
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the separate preparation of these two pure polynorbornene products by the same catalyst has not been reported

Method used

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  • Method for preparing norbornene open-loop translocation polymer or addition polymer
  • Method for preparing norbornene open-loop translocation polymer or addition polymer
  • Method for preparing norbornene open-loop translocation polymer or addition polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Ligand (C 6 h5 )N=CC 2 h 3 (CH 3 )C 6 h 2 (CH 3 ) Preparation of OH

[0033] in N 2 2.0g (11.4mmol) 7-hydroxy-3,4-dimethylindanone and 1.4mL (15.0mmol) aniline were added to a 100mL three-necked flask, then 30mL absolute ethanol, 0.1mL formic acid, 0.7 g 4A molecular sieve. Heat to reflux for 48 hours. After the end of the reaction, filter, collect the filtrate, and use anhydrous Mg 2 SO 4 It was dried, concentrated, and passed through a silica gel column with a mixed solution of petroleum ether and ethyl acetate as an eluent to obtain 2.3 g of a yellow solid with a yield of 80%.

Embodiment 2

[0034] Example 2 Ligand [C 6 h 3 -i-(C 3 h 7 ) 2 -2,6] N=CC 2 h 3 (CH 3 )C 6 h 2 (CH 3 ) Preparation of OH

[0035] in N 2 1.3mL (11.4mmol) TiCl will be dissolved within 30min 4 30 mL of toluene solution was added to 40 mL of toluene solution containing 8.6 mL (45.4 mmol) of 2,6-diisopropylaniline. The reaction mixture was then heated to 90° C., and 2 g (11.4 mmol) of 7-hydroxy-3,4-dimethylindanone was added after 30 min. At this temperature, the reaction was carried out for 48 hours. After the reaction, the reaction solution was poured into Na 2 CO 3 Saturated aqueous solution, liquid separation, organic phase with anhydrous Mg 2 SO 4 It was dried, concentrated, and passed through a silica gel column using a mixed solution of petroleum ether and ethyl acetate as an eluent to obtain 1.54 g of a red solid with a yield of 40%.

Embodiment 3

[0036] Example 3 Ligand (C 6 h 5 )N=CC 2 h 3 (CH 3 )C 6 h 2 (CH 3 )(C 4 h 9 ) Preparation of OH

[0037] in N 2 1.3mL (11.4mmol) TiCl will be dissolved within 30min 4 30mL of toluene solution was added to 40mL of toluene solution containing 4.3mL (45.4mmol) aniline. Then the reaction mixture was heated to 90° C., and 2.63 g (11.4 mmol) of 7-hydroxy-3,4-dimethyl-6-tert-butylindanone was added after 30 min. At this temperature, the reaction was carried out for 48 hours. After the reaction, the reaction solution was poured into Na 2 CO 3 Saturated aqueous solution, liquid separation, organic phase with anhydrous Mg 2 SO 4 It was dried, concentrated, and passed through a silica gel column using a mixed solution of petroleum ether and ethyl acetate as an eluent to obtain 2.75 g of an orange-red solid with a yield of 45%.

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PUM

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Abstract

The invention pertains to chemical industry, particularly relates to a norbornene ring-opening metathesis polymer and preparation of addition polymer. Catalyst system is composed of two portions of A and B, A portion is trivalent iridium catalyst in half-sandwich structure, which is represented by formula Cp*IrL, wherein Cp* represents ligand of 1,2,3,4,5-Pentamethylcyclopentadiene, L represents bidentate ligand containing O, N heteroatom which is capable of coordinating with late transition metal; B portion is represented by methylaluminoxane (MAO) or modidied methylaluminoxane (MMAO). A portion of the invention is simple to prepare, stable in air. Purified norbornene ring-opening metathesis polymer and catalysate of addition polymer can be respectively obtained by regulating proportion of A and B portion.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing norbornene ring-opening metathesis polymers and addition polymers with a novel semi-sandwich structure trivalent iridium catalyst. Background technique [0002] Norbornene and its derivatives can be polymerized in three ways, which are ring-opening metathesis polymerization, addition polymerization and cationic polymerization. Different polymerization methods give norbornene polymers with different structures and properties. There are usually two catalytic systems for ring-opening metathesis polymerization: one is composed of halides, oxides or oxidation-halides of metals such as tungsten, molybdenum, rhenium, ruthenium, and alkylating reagents and accelerators; the other is The first is a catalytic system composed of transition metal carbene compounds and some initiators. The resulting polymer chains still contain double bonds and c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/08C08F132/04C08F4/70
Inventor 金国新孟夏
Owner FUDAN UNIV
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