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Aza cyclic carbine rear earth catalyst for crystallinity 3,4-polyisoprene

A nitrogen-heterocyclic carbene and polyisoprene technology, which is applied in the field of nitrogen-heterocyclic carbene rare earth catalysts, can solve the problems of wear resistance degradation and other problems

Active Publication Date: 2008-04-09
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

However, the inherent dynamic viscoelastic properties of rubber make it impossible to avoid the increase of rolling resistance and heat generation and the decline of wear resistance while improving the traction performance of the tire.

Method used

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  • Aza cyclic carbine rear earth catalyst for crystallinity 3,4-polyisoprene
  • Aza cyclic carbine rear earth catalyst for crystallinity 3,4-polyisoprene
  • Aza cyclic carbine rear earth catalyst for crystallinity 3,4-polyisoprene

Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0039] Preparation Example 1 Complex 1 ((Flu-NHC) Y(CH 2 SiMe 3 ) 2 ) preparation, its process is as follows:

[0040]

[0041] In the glove box, place 0.035 g of LiCH 2 SiMe 3 Dissolve in 30mL of toluene, and add 0.168g of ligand (Flu-H-NHC-H)Br to it, react at room temperature for 3h, add the reaction solution to 20ml, 0.181g of Y(CH 2 SiMe 3 ) 3 (THF) 2 The reaction was continued for 5 h in a toluene solution, the toluene solution was concentrated to 2 ml, 2 ml of n-hexane was added, and recrystallized in a refrigerator at -30°C overnight to obtain complex 1 as yellow crystals. Wash with n-hexane and dry in vacuum for 2 hours to obtain 0.145 g. The yield was 61.7%. deuterated benzene (C 6 D. 6 ) was used as a reagent to characterize the structure of complex 1 by H-NMR spectroscopy and elemental analysis. 1 H NMR (400MHz, C 6 D. 6 , 25°C): δ-1.90, -1.59 (AB, 2 J H-H =10.8 Hz, 4H, Y-CH 2 SiMe 3 ), 0.22(s, 18H, Y-CH 2 SiMe 3 ), 1.85(s, 6H, C 6 h 2 Me ...

preparation Embodiment 2

[0042] Preparation Example 2 Complex 2 ((Flu-NHC)Ho(CH 2 SiMe 3 ) 2 ) preparation, its process is as follows:

[0043]

[0044] In the glove box, place 0.035 g of LiCH 2 SiMe 3 Dissolved in 30mL of toluene, and 0.168g ligand (Flu-H-NHC-H)Br was added to it, after 3h reaction at room temperature, the reaction solution was added to 30ml, 0.209g Ho(CH 2 SiMe 3 ) 3 (THF) 2 In the toluene solution, the reaction was continued for 6h, the toluene solution was concentrated to 2ml, 2ml of n-hexane was added, and recrystallized in a -30°C refrigerator overnight to obtain complex 2 as yellow crystals. Wash with n-hexane and dry in vacuo for 2 hours to obtain 0.164 g. The yield was 62.4%. The structure of complex 2 was characterized by elemental analysis, and its molecular formula is C 35 h 47 HoN 2 Si 2 . Among them, the carbon content is 57.53; the hydrogen content is 6.81; the nitrogen content is 3.16.

preparation Embodiment 3

[0045] Preparation Example 3 Complex 3 ((Flu-NHC)Lu(CH 2 SiMe 3 ) 2 ) preparation, its process is as follows:

[0046]

[0047] In the glove box, place 0.035 g of LiCH 2 SiMe 3 Dissolve in 30mL of toluene, and 0.168g ligand (Flu-H-NHC-H)Br was added to it, after reacting at room temperature for 6h, the reaction solution was added to 30ml, 0.213g Lu(CH 2 SiMe 3 ) 3 (THF) 2 The reaction was continued for 6 hours in a toluene solution, the toluene solution was concentrated to 2ml, 2ml of n-hexane was added, and recrystallized in a -30°C refrigerator overnight to obtain complex 3 as yellow crystals. Wash with n-hexane and dry to obtain 0.180g. The yield was 67.7%. deuterated benzene (C 6 D. 6 ) was used as a reagent to characterize the structure of complex 3 by H NMR spectroscopy and elemental analysis. 1 H NMR (400MHz, C 6 D. 6 , 25°C): δ-2.18, -1.90 (AB, 2 J H-H =10.8Hz, 4H, Lu-CH 2 SiMe 3 ), 0.22(s, 18H, Lu-CH 2 SiMe 3 ), 1.85(s, 6H, C 6 h 2 Me 3 ), 2....

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Abstract

The present invention relates to a nitrogen heterocyclic carbene rare earth complex, a catalyst system which consists of the present invention, aluminum alkyl and an organoboron salt can catalyse the isoprene to carry out the solution polymerization, so as to prepare the polyisoprene with the crystallization property, high 3, 4-structure and high glass transition temperature (Tg). The molar ratio of aluminum alkyl and the rare earth complex is within the scope of 1 to 100, the molar ratio of the organoboron salt and the rare earth complex is within the scope of 0.5 to 2.0; the solvent which is used for polymerization can be toluene, bromobenzene, n-hexane, dichloromethane or chlorobenzene; the polymerization temperature range is -20 DEG C to 80 DEG C, the reaction time of polymerization at minus 20 DEG C is 36 hours, the reaction time of polymerization at 80 DEG C is 1 hour, and the monomer conversion rate can be up to 100 percent. The reaction is characterized by active polymerization, the molecular weight of the product can be controlled by the molar ratio of the monomer and the catalyst, the molecular weight of the polyisoprene can achieve 360,000 at most, and the glass transition temperature Tg is equal to 5 DEG C to 50 DEG C. The content of the 3, 4 structure of the polyisoprene is affected by the spatial effect and the electronic effect of the rare earth complex, the solvent type for polymerization reaction and the polymerization reaction temperature and so on, which is changed between 76 percent and 99 percent.

Description

technical field [0001] The present invention relates to azacyclic carbene rare earth catalysts for crystalline 3,4-polyisoprene. Background technique [0002] Conjugated diolefins can be polymerized to obtain various polymers with stereoregular structures, many of which are synthetic rubbers with excellent performance, thus advancing rubber synthesis technology to a new stage, making the structure of synthetic rubber, product quality and quantity all There have been major reforms and growth. Isoprene rubber is referred to as isoprene rubber (IR), which is mainly divided into three categories: cis 1,4-IR, trans 1,4-IR, and 3,4-IR. cis 1,4-IR is a general-purpose synthetic rubber, which can replace natural rubber because its molecular structure and properties are very similar to natural rubber. Reverse 1,4-IR is also known as synthetic eucommia rubber or balata rubber. It exists as a crystalline polymer at room temperature and has been developed for medical materials and sha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/08C08F4/602
Inventor 崔冬梅王保力
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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