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Supported iron catalyst, preparation method thereof and iron catalyst system

An iron catalyst and supported technology, applied in the field of olefin polymerization catalysts, can solve the problems of high cost, high price and harsh use conditions of olefin polymerization, and achieve the effects of high polymerization activity, wide applicability and good shape.

Active Publication Date: 2017-12-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when this type of catalyst is not supported, the obtained polymer is in an amorphous state and cannot be used in the widely used slurry or gas phase polymerization process.
[0003] At present, there are many reports on the loading of single active site catalysts, among which silica gel is the most reported research (CN1174848A, CN1174849A, CN1356343A, US4,808,561, US5,026,797, US5,763,543, US5,661,098). Type catalysts can be used in some polymerization processes, but the use conditions are relatively harsh, and usually require expensive methyl aluminoxane (MAO) as a cocatalyst, which makes the cost of olefin polymerization higher
[0004] There are also literature reports (such as Acta Polymer Sinica, 2004 (3), 406-409), using zinc dichloride and MAO to process silica gel in the Ziegler-Natta catalyst system, compared to the catalyst without adding zinc dichloride, Its activity is improved, but the molecular weight and distribution of the polymer change greatly, and the processing performance of the polymer cannot be effectively controlled

Method used

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  • Supported iron catalyst, preparation method thereof and iron catalyst system
  • Supported iron catalyst, preparation method thereof and iron catalyst system
  • Supported iron catalyst, preparation method thereof and iron catalyst system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] This example is used to illustrate the supported iron catalyst of the present invention and its preparation method.

[0069] 1) Preparation of zinc chloride / silica gel carrier

[0070] Under nitrogen protection, in a glass reactor, add 0.54 g of zinc chloride at room temperature, then add 500 ml of tetrahydrofuran, start stirring, add 13.16 g of silica gel into the reactor, raise the temperature to 65 ° C, stir and dissolve for 2 hours, and then The solvent was evaporated at 80°C to give a white solid powder. The white solid powder was vacuum-dried at 100°C for 2 hours, and then vacuum-dried at 300°C for 10 hours to obtain a solid zinc chloride / silica gel carrier with good fluidity. According to gas chromatography analysis, no tetrahydrofuran was detected.

[0071] 2) Loading of iron single-site catalysts

[0072] Under nitrogen protection, 1.4 grams of the zinc chloride / silica gel carrier prepared above was added to a glass reactor, 20 milliliters of toluene was adde...

Embodiment 2

[0074] This example is used to illustrate the supported iron catalyst of the present invention and its preparation method.

[0075] 1) Preparation of zinc chloride / silica gel carrier

[0076] Under nitrogen protection, in a glass reactor, add 0.67 g of zinc chloride at room temperature, then add 500 ml of tetrahydrofuran, start stirring, add 10.5 g of silica gel into the reactor, raise the temperature to 65 ° C, stir and dissolve for 2 hours, and then The solvent was evaporated at 80°C to give a white solid powder. The white solid powder was vacuum-dried at 100°C for 2 hours, and then vacuum-dried at 300°C for 10 hours to obtain a solid zinc chloride / silica gel carrier with good fluidity. According to gas chromatography analysis, no tetrahydrofuran was detected.

[0077] 2) Loading of iron single-site catalysts

[0078] Under nitrogen protection, 1.1 grams of the zinc chloride / silica gel carrier prepared above was added to a glass reactor, 20 milliliters of toluene was added...

Embodiment 3

[0080] This example is used to illustrate the supported iron catalyst of the present invention and its preparation method.

[0081] 1) Preparation of zinc chloride / silica gel carrier

[0082]Under nitrogen protection, in a glass reactor, add 1.2 grams of zinc chloride at room temperature, then add 500 milliliters of tetrahydrofuran, start stirring, add 13.08 grams of silica gel into the reactor, raise the temperature to 65 ° C, stir and dissolve for 2 hours, and then The solvent was evaporated at 80°C to give a white solid powder. The white solid powder was vacuum-dried at 100°C for 2 hours, and then vacuum-dried at 300°C for 10 hours to obtain a solid zinc chloride / silica gel carrier with good fluidity. According to gas chromatography analysis, no tetrahydrofuran was detected.

[0083] 2) Loading of iron single-site catalysts

[0084] Under nitrogen protection, 1.1 grams of the zinc chloride / silica gel carrier prepared above was added to a glass reactor, 20 milliliters of t...

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Abstract

The invention belongs to the field of olefin polymerization catalysts and particularly provides a supported iron catalyst, a preparation method thereof and an iron catalyst system. The supported iron catalyst comprises a zinc chloride / silica gel carrier and an iron single active center component supported by the carrier, wherein a precursor of the iron single active center component is a bis(imino)pyridine Fe (II) complex with a structure as shown in the formula 1, wherein R1-R10 are same or different and are respectively selected from H, halogens or C1-C4 straight-chain or branch-chain alkyls. Compared with a bis(imino)pyridine Fe (II) catalyst which is not modified by zinc chloride, the supported iron catalyst provided by the invention is not only relatively high in polymerization activity, but also capable of basically keeping the molecular weight distribution of a polymer constant when being used for olefin polymerization.

Description

technical field [0001] The invention belongs to the field of olefin polymerization catalysts, and in particular relates to a supported iron catalyst, a preparation method thereof, and an iron catalyst system for olefin polymerization. Background technique [0002] In the development of olefin polymerization catalysts, single-site catalysts developed in the 1990s have received great development and attention. In particular, iron and cobalt metal complexes containing pyridinediimine ligands have high catalytic activity for olefin oligomerization and polymerization, and can obtain functionalized polyolefin resins, which have good application prospects. However, when this type of catalyst is not supported, the obtained polymer is in an amorphous state, which cannot be used in the widely used slurry method or gas phase polymerization process. [0003] At present, there are many reports on the loading of single active site catalysts, among which silica gel is the most reported re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F4/70C08F4/02
CPCC08F110/02C08F4/7042C08F4/025
Inventor 刘东兵刘雨平李岩高榕周俊领
Owner CHINA PETROLEUM & CHEM CORP
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