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Highly branched iron-based conjugated diene polymer and preparation method thereof

A technology of conjugated diene and polymer, which is applied in the field of highly branched iron-based conjugated diene polymer and its preparation, can solve the problems of high reaction toxicity, high gel content, poor solubility, etc., and achieve a wide range of molecular weight distribution , optimize the production process, improve the effect of processing performance

Pending Publication Date: 2022-03-29
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Wang Fosong's research group prepared polyisoprene with high 3.4-structure content, but the gel content of the polymer is high, up to 10%, which affects the processing performance of the product
Moreover, the system reacts in an aromatic solvent at low temperature, and the reaction toxicity is high, which does not meet the production requirements of green chemistry.
Giovanni Ricci et al. using a bidentate ligand / FeCl 2 / MAO catalyst system, prepared highly branched isoprene polymer, but there are few reports on the iron-catalyzed copolymerization of isoprene and butadiene
Moreover, in this catalytic system, the catalyst reacts in the form of a suspension, and the poor solubility will lead to difficulties in feeding materials for continuous production, and the use of MAO aluminum reagents is costly, so it does not meet the requirements of industrial production.
Therefore, there are still great limitations in promoting the industrial production of highly branched polyconjugated dienes.

Method used

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  • Highly branched iron-based conjugated diene polymer and preparation method thereof
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  • Highly branched iron-based conjugated diene polymer and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1: the structural formula of bipyridyl iron complex (catalyst 1) is:

[0049]

[0050] The preparation method is as follows: under an argon atmosphere, firstly bake a 25mL Schlenk tube three times, and then add 20mL redistilled cyclohexane, 0.2mmol Fe(2-EHA) 3 and 0.2mmol N,N-bidentate electron-rich compound L1, stirred and reacted at room temperature for 1h to obtain a brownish-yellow liquid, that is, a bipyridyl iron complex solution.

[0051] Mass Spectrometry: C 34 h 53 FeN 2 o 6: [M+H] + : Theoretical value: 641.3253; measured value: 641.3257.

[0052] Elemental Analysis: C 34 h 53 FeN 2 o 6 : Theoretical value: C, 63.64%; H, 8.33%; N, 4.37%; Found value: C, 63.59%; H, 8.37%; N, 4.33%.

Embodiment 2

[0053] Embodiment 2: the structural formula of bipyridyl iron complex (catalyst 2) is:

[0054]

[0055] The preparation method is as follows: under an argon atmosphere, firstly bake a 25mL Schlenk tube three times, and then add 20mL redistilled cyclohexane, 0.2mmol Fe(2-EHA) 3 and 0.2mmol N,N-bidentate electron-rich compound L2, stirred and reacted at room temperature for 1h to obtain a brownish-yellow liquid, that is, a bipyridyl iron complex solution.

[0056] Mass Spectrometry: C 36 h 53 FeN 2 o 6: [M+H] + : Theoretical value: 665.3253; measured value: 665.3256.

[0057] Elemental Analysis: C 36 h 53 FeN 2 o 6 : Theoretical value: C, 64.96%; H, 8.03%; N, 4.21%; Found value: C, 64.93%; H, 8.09%; N, 4.27%.

Embodiment 3

[0058] Embodiment 3: the structural formula of bipyridyl iron complex (catalyst 3) is:

[0059]

[0060] The preparation method is as follows: under an argon atmosphere, firstly bake a 25mL Schlenk tube three times, and then add 20mL redistilled cyclohexane, 0.2mmol Fe(2-EHA) 3 and 0.2mmol N,N-bidentate electron-rich compound L3, stirred and reacted at room temperature for 1h to obtain a brownish-yellow liquid, that is, a bipyridyl iron complex solution.

[0061] Mass Spectrometry: C 36 h 57 FeN 2 o 6: [M+H] + : Theoretical value: 669.3566; measured value: 669.3571.

[0062] Elemental Analysis: C 36 h 57 FeN 2 o 6 : Theoretical value: C, 64.57%; H, 8.58%; N, 4.18%; Found value: C, 64.63%; H, 8.52%; N, 4.23%.

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Abstract

The invention provides a high-branch-chain iron-based conjugated diene polymer and a preparation method thereof, and belongs to the field of conjugated diene catalytic polymerization. In the iron-based conjugated diene polymer provided by the invention, the proportion of a 3, 4-(1, 2-) structure is 60%-80%, the proportion of a 1, 4 structure is 20%-40%, and the gel content is 1t; and the glass transition temperature is-80 DEG C to 10 DEG C. The solubility of the iron complex in a reaction solvent is remarkably improved by changing anions in the iron complex, the modified aluminum reagent obtained by reacting the modifier with aluminum alkyl is matched with the iron complex, the reaction activity is excellent, and compared with the prior art, the use of a necessary dealkylation reagent in an aluminum alkyl system is avoided; the technological process is reduced, the reaction cost is reduced, and important technical support is provided for industrial production of the iron-based rubber. The obtained conjugated diene polymer has the characteristics of high branching, low gel content, even no gel and low glass transition temperature, and the product quality and performance are remarkably improved.

Description

technical field [0001] The invention belongs to the field of catalytic polymerization of conjugated dienes, and in particular relates to a highly branched iron-based conjugated diene polymer and a preparation method thereof. Background technique [0002] Artificially synthesized highly branched polyconjugated diene is an ideal compound for high-performance environmental protection tires. It has excellent wet skid resistance, low rolling resistance, low compression heat generation and high anti-aging performance. Therefore, it is increasingly favored by the rubber industry. More favors. When high-branched pentamethylene rubber is used as tire support rubber, it can significantly improve the tire's anti-wet skid performance without increasing the tire rolling resistance, and can greatly reduce the compression heat of the tire. It is called "China The potential eighth type of synthetic rubber" has great application prospects in high-performance tires such as aviation tires and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F136/08C08F136/06C08F236/06C08F236/08
CPCC08F4/7006C08F136/08C08F136/06C08F236/06C08F236/08
Inventor 王庆刚王亮匡佳陈小羽周丽
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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