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A kind of α-imine iron/cobalt complex catalyst and its preparation and use

A technology of catalysts and complexes, applied in the field of α-imine iron/cobalt complex catalysts and their preparation, to achieve stable performance, good catalytic activity, and simple operating conditions

Active Publication Date: 2022-04-29
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] It can be seen that, in terms of catalyzing the polymerization of isoprene, the catalytic activity and selectivity need to be improved, and it is urgent to develop a catalytic system that can not only ensure the catalytic activity but also significantly improve the catalytic selectivity.

Method used

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  • A kind of α-imine iron/cobalt complex catalyst and its preparation and use
  • A kind of α-imine iron/cobalt complex catalyst and its preparation and use
  • A kind of α-imine iron/cobalt complex catalyst and its preparation and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0120] [2-(1-(1-naphthylamine) ethyl) pyridine] ferrous chloride [complex Fe1] shown in preparation formula Ⅰ-1:

[0121] At room temperature, the FeCl 2 4H 2 O (0.20g, 1.00mmol) and 2-(1-(1-naphthylamine)ethyl)pyridine (L1, 0.27g, 1.15mmol) were mixed and dissolved in ethanol, stirred for 12 hours under nitrogen protection, and removed under reduced pressure After ethanol was added to diethyl ether, a blue solid precipitated out, filtered, washed with diethyl ether, and dried to obtain a blue solid. Yield: 75%.

[0122] The structural confirmation data are as follows:

[0123] FT-IR (KBr, cm -1 ):3448(s), 3058(m), 2968(w), 1918(w), 2853(w), 1630(νC=N,s), 1595(s), 1573(w), 1508(m) ,1438(m),890(w),1369(s),1340(w),1262(m),1254(m),1227(w),1164(w),1126(w),1078(w) , 1016(w), 975(w), 870(w), 813(w), 766(s), 746(w), 735(w).

[0124] Elemental Analysis: C 34 h 28 Cl 2 FeN 4 (619.37) Theoretical value: C, 65.93, H, 4.56, N, 9.05. Experimental value C, 66.24, H, 4.90, N, 8.69...

Embodiment 2

[0126] [2-(1-(2-methyl)-naphthylamine) ethyl) pyridine] ferrous chloride [complex Fe2] shown in preparation formula I-2:

[0127] At room temperature, the FeCl 2 4H 2 O (0.20g, 1.00mmol) and 2-(1-(2-methyl)-naphthylamine)ethyl)pyridine (L2, 0.30g, 1.15mmol) were mixed and dissolved in ethanol, and stirred for 12 hours under nitrogen protection After removing ethanol under reduced pressure, an orange solid was precipitated by adding ether, which was filtered, washed with ether, and dried to obtain an orange solid. Yield: 76%.

[0128] The structural confirmation data are as follows:

[0129] FT-IR (KBr, cm -1):3448(s), 3059(m), 2917(m), 1619(νC=N,s), 1592(s), 1570(w), 1507(w), 1440(m), 1372(s) ,1341(s),1316(w),1257(m),1234(w),1163(w),1129(w),1015(m),868(m),813(s),780(s) ,766(m),743(m).

[0130] Elemental Analysis: C 36 h 32 C l2 FeN 4 (647.43) Theoretical value: C, 66.79, H, 4.98, N, 8.65. Experimental value: C, 66.52, H, 4.78, N, 8.71.

Embodiment 3

[0132] [2-(1-(2-(1-phenylethyl)-naphthylamine) ethyl) pyridine] ferrous chloride [complex Fe3] shown in preparation formula I-3:

[0133] At room temperature, the FeCl 2 4H 2 O (0.02g, 0.10mmol) and 2-(1-(2-(1-phenylethyl)-naphthylamine)ethyl)pyridine (L3, 0.04g, 0.11mmol) were mixed and dissolved in ethanol, under nitrogen protection Stir under low pressure for 12 hours, remove ethanol under reduced pressure, add diethyl ether, a blue solid precipitates out, filter, wash with diethyl ether, and dry to obtain a blue solid. Yield: 65%.

[0134] The structural confirmation data are as follows:

[0135] FT-IR (KBr, cm -1 ):2970(s), 2905(s), 1620(νC=N,m), 1592(s), 1569(w), 1491(w), 1444(w), 1418(w), 1372(s) ,1310(s),1256(s),1158(w),1056(s),1021(w),974(w),903(w),866(s),830(m),809(w) ,772(m),746(s),702(s).

[0136] Elemental Analysis: C 50 h 44 C l2 FeN 4 (827.68) Theoretical value: C, 72.56, H, 5.36, N, 6.77. Experimental value: 73.00, H, 4.92, N, 6.72.

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Abstract

The invention discloses an α-imine iron / cobalt complex catalyst, its preparation and application, and belongs to the technical field of polyolefin catalysts. The present invention utilizes a specific α-imine ligand and iron or cobalt center metal to construct a complex catalyst. This type of complex catalyst has a single catalytic active center, and can adjust the molecular weight of the polymer and its microscopic molecular structure by adjusting the structure of the ligand and the polymerization conditions. It has the advantages of high catalytic activity, low cost, and stable performance. , has great application prospects in industrial production.

Description

technical field [0001] The invention belongs to the technical field of polyolefin catalysts, and in particular relates to an α-imine iron / cobalt complex catalyst and its preparation and application. Background technique [0002] Synthetic rubber is one of the three major synthetic materials in the world today, and its output is second only to synthetic resin (or plastic) and synthetic fiber. Polyisoprene has the same monomer structure as natural rubber, so it occupies a pivotal position in the field of synthetic rubber materials. Natural rubber is very sensitive to the longitude, latitude and climate of the planting area, and is restricted by the inability to expand production and occupy the grain planting area, so its output is far from meeting social needs. According to statistics from the Association of Natural Rubber Producing Countries (ANRPC) and the International Rubber Organization (IRSG), my country's natural rubber consumption has exceeded 4.5 million tons in 2016...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/70C08F136/08C07F15/02C07F15/06
CPCC08F136/08C07F15/025C07F15/065C08F4/7006
Inventor 张丽平孙文华付少海林文华
Owner JIANGNAN UNIV
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