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Olefin polymerization catalyst containing beta-diketone metal complex, preparation and application thereof

A metal complex and olefin polymerization technology, which is applied in the field of olefin polymerization catalysts containing β-diketone metal complexes and its preparation and application, and can solve the problems of rare olefin polymerization catalysts

Active Publication Date: 2013-02-13
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(Organometallics 2008, 27, 3642-3653; J Polym Sci Polym Chem, 2008, 46, 2038-2048) However, olefin polymerization catalysts of supported β-diketone IVB and VB metal complexes are still rare

Method used

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  • Olefin polymerization catalyst containing beta-diketone metal complex, preparation and application thereof
  • Olefin polymerization catalyst containing beta-diketone metal complex, preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 35.0mmol potassium carbonate and 70.0mmol potassium iodide into a 500mL three-neck flask, under a nitrogen atmosphere and electromagnetic stirring, add the acetone solution of acetylacetone (75.0mmol acetylacetone is dissolved in 100mL acetone solution) and keep warm at 40-65°C 20 minutes. Then, add an acetone solution of 4-chloromethylstyrene (70.0mmol 4-chloromethylstyrene is dissolved in 40mL acetone), and react under a nitrogen atmosphere at a temperature of 50-80° C. for 12-24 hours. After the reaction was finished, the acetone was removed by rotary evaporation. The product was dissolved in 100 mL of ether, washed with 50 mL of distilled water to remove potassium carbonate and potassium iodide, and the washing was repeated 5 times. Ether was removed by rotary evaporation, and 14.1 g of yellow oily substance A was obtained by drying 1 [3-(4-vinylbenzyl)-2,4-pentanedione, its structure is shown in formula I, wherein R 1 =CH 3 , R 2 = H, R 3 =CH 3 ], yield ...

Embodiment 2

[0023] Replace the acetylacetone in Example 1 with 1,1,1,5,5,5-hexafluoroacetylacetone, and the operation is the same as in Example 1. Obtained 21.6 g of yellow oily substance A 2 [3-(4-vinylbenzyl)-1,1,1,5,5,5-hexafluoro-2,4-pentanedione, its structure is shown in formula I, wherein R 1 = CF 3 , R 2 = H, R 3 = CF 3 ], yield 95%.

Embodiment 3

[0025] Synthesis of poly[3-(4-vinylbenzyl)-2,4-pentanedione]-co-polystyrene caged polymer microspheres containing β-diketone ligands (A / B monomer molar ratio is 1:1).

[0026] Add 5.0 mmol of methacrylic acid and 50-150 mL of water into the flask, and stir to dissolve. With stirring, 50.0 mmol of styrene and 2.0 mmol of potassium, sodium or ammonium persulfate were added. Dissolved oxygen in the reaction solution was removed by passing nitrogen gas, and the flask was placed in a water bath at 60-90° C., and reacted for 12-24 hours under a nitrogen atmosphere. After the reaction, centrifuge, wash with water, and dry to obtain 5.0 g of polystyrene-co-polymethacrylic acid microspheres. Get 1.0g of polystyrene-co-polymethacrylic acid microspheres and disperse them in 100mL of water, then add 0.48mmol of potassium persulfate, sodium persulfate or ammonium persulfate, 12.0mmol of β-diketone prepared according to Example 1 Ligand Alkene A 1 , 12.0 mmol of styrene and 1.2 mmol of ...

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Abstract

The invention relates to an olefin polymerization catalyst containing beta-diketone metal complex, its preparation and application. The preparation comprises the following steps: letting potash, potassium iodide, acetylacetone, an acetone solvent of 2,2,6,6-tetramethyl-3,5-heptadione or 1,1,1,5,5,5-hexafluoroacetylacetone, and an acetone solvent of 4-chloromethyl styrene be subject to reaction toobtain an olefin monomer A containing beta-diketone dentate; dispersing template high-molecular microballoons in water, adding the olefin monomer A containing beta-diketone dentate, a copolyolefin monomer B, potassium persulfate, sodium peroxydisulfate or ammonium persulfate and divinylbenzene for copolymerization to obtain cage high-molecular microballoons containing beta-diketone ligand; and adding titanium tetrachloride, zirconium tetrachloride or vanadium tetrachloride at the temperature of -10 to -80 DEG C to obtain the cage high-molecular microballoon loading olefin polymerization catalyst containing beta-diketone metal complex. According to the invention, the spacing steric hindrance of the ligand, and the contact frequency and catalytic activity of the catalyst are improved.

Description

technical field [0001] The present invention relates to a cage polymer microsphere containing β-diketone ligand and its supported IVB and VB metal complex olefin polymerization catalyst and its preparation method, as well as the application of the catalyst in the polymerization of styrene and ethylene application. Background technique [0002] β-diketone and its derivatives can form complexes with IVB and VB metals such as titanium, zirconium, nickel and vanadium. These β-diketone metal complexes can be used as catalysts for olefin polymerization, and have a wide range of applications in styrene syndiotactic polymerization, norbornene ring-opening polymerization, and ethylene polymerization. Compared with Ziegler-Natta catalysts and metallocene catalysts, β-diketone organometallic complex olefin catalysts have the characteristics of high reactivity, weak oxophilicity and wide range of structure adjustment, and are an important research direction of olefin polymerization cat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/00C08F4/76C08F4/02C08F4/651C08F4/649C08F4/68C08F112/08C08F110/02
Inventor 王达张望清兰阳
Owner PETROCHINA CO LTD
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