Neodymium (Nd)-based homogeneous rare earth catalyst as well as preparation method and application thereof

A rare earth catalyst and catalyst technology are applied in the field of neodymium-based homogeneous rare earth catalyst and its preparation, which can solve the problems of environmental pollution and equipment corrosion, and achieve the effects of excellent physical and mechanical properties and stable and easy polymerization process.

Active Publication Date: 2011-06-29
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of halogen (such as chlorine) in the catalyst preparation process, it is highly corrosive to equipment and easily causes environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Starting from neodymium trioxide, using cyclohexane as solvent, adopting direct extraction method to obtain neodymium naphthenate / cyclohexane solution, wherein the concentration of neodymium [Nd 3+ ] is 0.21 mol / l. Triisobutylaluminum and diethylaluminum chloride were respectively prepared into cyclohexane solutions with a concentration of 2 mol / l for future use. The water value of the solvent is lower than 20ppm, and the oxygen is exhausted with nitrogen before use; the aging tank is dried and oxygenated.

[0042] Under the protection of nitrogen, add 630ml of cyclohexane solution to the 2L catalyst aging kettle, then add 30ml of isoprene and 62ml of neodymium naphthenate solution into the aging kettle, and then add 16ml of a Add the diethylaluminum chloride solution into the aging kettle, make isoprene, neodymium naphthenate and diethylaluminum chloride contact and react at 50°C for 7 minutes, then add 130ml of triisobutylaluminum solution, Aging at ℃ for 40 minutes...

Embodiment 2

[0045] Triisobutylaluminum and diethylaluminum chloride were respectively prepared into hexane solutions with a concentration of 0.5 mol / l for future use. Neodymium naphthenate is prepared into a hexane solution with a concentration of 0.21mol / l for later use. The treatment mode of the solvent and the aging tank is the same as in Example 1.

[0046] Under the protection of nitrogen, add 218ml of isoprene, 130ml of neodymium naphthenate solution and 8.0L of hexane solution into the 20L catalyst aging kettle, then add 190ml of diethylaluminum chloride solution at 0°C under stirring conditions, After contact reaction at 0° C. for 60 minutes, 546 ml of triisobutylaluminum solution was added, and aging continued for 10 hours. The catalyst concentration is 0.3×10 -5 mol / ml.

[0047] Under the protection of nitrogen, 350 g of isoprene, 1800 g of hexane and 340 ml of catalyst were successively added into a 5 L polymerization kettle, and the monomer concentration was 15%. After rea...

Embodiment 3

[0049] Diisobutylaluminum hydride and diethylaluminum chloride were respectively prepared into hexane solutions with a concentration of 0.5 mol / l for future use. Neodymium naphthenate is prepared into a hexane solution with a concentration of 0.21mol / l for later use. The treatment mode of the solvent and the aging tank is the same as in Example 1.

[0050] Under nitrogen protection, add 15ml of isoprene, 1.1L of hexane solution, 31ml of neodymium naphthenate solution into the 2L catalyst aging kettle, and then add 39ml of diethylaluminum chloride solution at 10°C under stirring conditions, After 20 minutes of contact reaction, 130 ml of triisobutylaluminum solution was added, and aging continued for 2 hours. The catalyst concentration is 0.5×10 -5 mol / ml.

[0051] Under the protection of nitrogen, 350 g of isoprene, 1800 g of hexane and 180 ml of catalyst were successively added into a 5 L polymerization kettle, and the monomer concentration was 15.4%. After reacting at 25...

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Abstract

The invention relates to a novel neodymium (Nd)-based homogeneous rare earth catalyst as well as a preparation method and application thereof in conjugated diene polymerization. The synthesis method of the catalyst is simple and easy to control, and the homogeneous and stable catalyst with high activity can be obtained by utilizing the method. By utilizing the Nd-based homogeneous rare earth catalyst, a conjugated diene polymer can be synthesized, wherein, the cis-structure content of the polymer is more than 98%, the weight-average molecular weight of the polymer can be adjusted within the range of 1,000,000-2,500,000, and the molecular weight distribution (MWD) ranges from 3.0 to 4.0; and the polymerization process is stable and easy to control, thus being applicable to continuous technological operation.

Description

Technical field: [0001] The invention relates to a rare earth catalyst, in particular to a novel neodymium homogeneous rare earth catalyst and a preparation method thereof. The neodymium-based homogeneous rare-earth catalyst of the invention is especially suitable as a catalyst for the polymerization of conjugated dienes to synthesize polymers with high cis-structure content. technical background: [0002] Conjugated diolefins undergo directional polymerization under the action of rare earth catalysts, and polymers with high cis structure content (>96%) and high molecular weight (such as polybutadiene and polyisoprene) can be synthesized. The polyisoprene rubber catalyzed by the rare earth catalyst is superior to the polyisoprene rubber catalyzed by the titanium catalyst in terms of microstructure and physical and mechanical properties, and its microstructure and macrostructure are closest to natural rubber, which is the closest natural rubber. Ideal replacement. Compar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F36/04C08F4/52
Inventor 张杰华炜谭金枚李传清梁爱民李洪泊李伟赵西明徐林于国柱欧阳素芳杨亮亮
Owner CHINA PETROLEUM & CHEM CORP
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