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Clamp-type iron complex and preparation method and application thereof

An iron complex and clamp-type technology, which is applied in the field of catalysis, can solve the problems of difficult preparation, expensive boron additives, and high price, and achieve the effects of easy control of the reaction, stable catalytic performance, and convenient preparation

Inactive Publication Date: 2012-08-15
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In recent years, a series of patents have disclosed catalysts that can be used for the selective polymerization of butadiene, such as the invention patent of application number 200710056309.2 and the invention patent of application number 200810050666.2, which have introduced rare earth catalysts that can be used for the selective polymerization of butadiene; but The catalysts reported in these patents either use expensive rare earth elements or expensive boron additives, and are not easy to prepare

Method used

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  • Clamp-type iron complex and preparation method and application thereof
  • Clamp-type iron complex and preparation method and application thereof
  • Clamp-type iron complex and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 Preparation of pincer iron complex (iron complex 1)

[0034]

[0035] At -78°C to -40°C, a hexane solution of butyllithium (1.2mL, 1.88mmol) was slowly added dropwise to 2,6-bis(N-phenyl)iminobromobenzene (0.6690g , 1.84mmol) in 30mL tetrahydrofuran solution, add FeCl to it after 30 minutes of low temperature reaction 2 (0.2332g, 1.88mmol), naturally rise to room temperature and continue to react for 12 hours, stop the reaction, concentrate the reaction solution to about 5ml, add about 15ml of hexane, filter out insoluble matter, and place the filtrate in a refrigerator at -30°C after concentration Freeze overnight to obtain 0.6200 g of purple crystalline compound with a yield of 60%. Elemental analysis, its molecular formula is C 28 h 31 Cl 2 FeLiN 2 O2 (%): C, 59.92; H, 5.57; Cl, ​​12.63; N, 5.86; Fe, 9.95;

Embodiment 2

[0036] Example 2 Preparation of pincer iron complex (iron complex 2)

[0037]

[0038] Under the condition of -78℃~-40℃, a hexane solution of butyllithium (1.2mL, 1.88mmol) was slowly added dropwise to 2,6-bis(N-2,6-dimethylphenyl) Aminobromobenzene (0.7716, 1.84mmol) in 30mL tetrahydrofuran solution, reacted at low temperature for 30 minutes, then added FeCl 2 (0.2332g, 1.84mmol), naturally rise to room temperature and continue to react for 12 hours, stop the reaction, concentrate the reaction solution to about 5ml, add about 15ml of hexane, filter out insoluble matter, and place the filtrate in a refrigerator at -30°C after concentration After freezing overnight, 0.7724 g of a purple crystalline compound was obtained, with a yield of 68%. Elemental analysis, its molecular formula is C 32 h 39 Cl 2 FeLiN 2 o 2 (%): C, 62.26; H, 6.37; Cl, ​​11.49; Fe, 9.05; Li, 1.12; N, 4.54;

Embodiment 3

[0039] Example 3 Preparation of pincer iron complex (iron complex 3)

[0040]

[0041] At -78°C to -40°C, a hexane solution of butyllithium (1.2mL, 1.88mmol) was slowly added dropwise to 2,6-bis(N-2,6-diethylphenyl) Aminobromobenzene (0.8748, 1.84mmol) in 30mL tetrahydrofuran solution, reacted at low temperature for 30 minutes, then added FeCl 2 (0.2332g, 1.84mmol), naturally rise to room temperature and continue to react for 12 hours, stop the reaction, concentrate the reaction solution to about 5ml, add about 15ml of hexane, filter out insoluble matter, and place the filtrate in a refrigerator at -30°C after concentration After freezing overnight, 0.8922 g of a purple crystalline compound was obtained with a yield of 72%. Elemental analysis, its molecular formula is C 36 h 47 Cl 2 FeLiN 2 o 2 (%): C, 64.20; H, 7.03; Cl, ​​10.53; Fe, 8.29; Li, 1.03; N, 4.16; O, 4.75.

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Abstract

The invention discloses a clamp-type iron complex and a preparation method and application thereof, and belongs to the field of catalysis technologies. The clamp-type iron complex is based on [NCN]-coordination. The preparation method comprises the following steps of: adding a butyl lithium solution into a ligand solution under the condition of the temperature of -78 to -40 DEG C, and reacting to obtain a reaction solution; adding ferrous chloride into the reaction solution, naturally raising the temperature to room temperature, and continuing reaction; and adding hexane to perform filtration and recrystallization. A catalyst consisting of the [NCN]-coordination clamp-type iron complex and alkyl aluminum is used for catalyzing butadiene syn-1,4 to perform selective polymerization. The clamp-type iron complex is convenient to prepare and high in stability; during selective polymerization of the butadiene under the catalyst, the using amount of the catalyst is small, the polymerization reaction speed is high, the conversion efficiency is high, and syn-1,4 selectivity is relatively high, and polymer molecule weight and molecule weight distribution are controllable; the system formed by the catalyst is homogeneous; the clamp-type iron complex is convenient to use; during polymerization, the temperature fluctuation range is small; and the reaction is easy to control.

Description

technical field [0001] The invention belongs to the field of catalytic technology, in particular to a method based on [NCN] - Coordinated pincer iron complexes, their synthesis and their use in the cis-1,4-selective polymerization of butadiene. Background technique [0002] At present, polyolefin materials have become a polymer raw material with the largest output and the most extensive uses in synthetic resins. Among them, polybutadiene and polyisoprene are important synthetic rubber varieties. Polybutadiene rubber is the second largest general-purpose synthetic polymer material in the world after styrene-butadiene rubber. It has the advantages of excellent elasticity, strong wear resistance, low temperature resistance, low heat generation, small hysteresis loss, flex resistance, crack resistance and good dynamic performance. It can be used with natural rubber, neoprene and nitrile rubber, etc. Comparable, it has a wide range of applications in the production of rubber p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/02C08F4/70C08F36/06
Inventor 母瀛张敬顺高伟
Owner JILIN UNIV
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