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Carried catalyzer for olefinic polymerization and preparation method

An olefin polymerization and catalyst technology is applied in the field of supported olefin polymerization catalyst and its preparation, and achieves the effects of excellent ion exchange performance, large pore size and good shape.

Inactive Publication Date: 2004-05-26
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, metallocene catalysts are mostly supported by SiO 2 as a support, and the research on the support of late transition metal olefin polymerization catalysts is still rarely reported

Method used

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  • Carried catalyzer for olefinic polymerization and preparation method
  • Carried catalyzer for olefinic polymerization and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of the catalyst: Add 1.0000g (6.13mmol) of 2,6-diacetylpyridine into a 100mL Schlenk bottle equipped with a stirring magnet, and inject 14.9196g into the reactor equipped with a stirring magnet with a syringe under the protection of argon. (24.52mmol, 4equiv.) 2,6-Diisopropylaniline, 80mL anhydrous methanol and 0.2mL formic acid, react at 60°C for 48h. Cool, filter, and wash with cold methanol to obtain a yellow powdery product. After drying, it was extracted with isopropanol for 24 hours to remove the monoimine by-product, and a light yellow powdered ligand was obtained. Weigh a certain amount of ligand (1.05equiv.) into a 20mL Schlenk bottle equipped with a magnetic stirrer, and add FeCl 2 ·4H 2 O(1.00equiv.). Evacuate and ventilate with argon three times, inject 10 mL of dry tetrahydrofuran under the protection of argon, and react at 25°C for 2 h. After the reaction, 5 mL of n-pentane was added, then filtered, washed with n-pentane and anhydrous ether, and dr...

Embodiment 2

[0034] Preparation of the catalyst: the same as in Example 1.

[0035] Preparation of carrier precursor: CaO, SiO 2 , K2 O, H 2 O was put into a stainless steel reactor at a weight ratio of 1:1:1.5:1000, and crystallized at 500°C for 25 days to obtain a carrier precursor molecular sieve calcium silicon compound.

[0036] Preparation of supported catalyst: After 5g of molecular sieve calcium silicon compound was vacuum dried at 30°C for 10 hours, 20mL of 1.8mol / L triethylaluminum toluene solution was added, stirred at 50°C for 6 hours, filtered, and heated with anhydrous toluene Washing and filtering, 20mL each time, washing three times in total, after filtering and drying to prepare molecular sieve-like calcium silicate compound carrier. 0.25 g of catalyst Ia was added to the above system and stirred at 40° C. for 10 hours. Wash with toluene several times until the supernatant becomes colorless. Vacuum dry and store under inert gas for later use.

[0037] Ethylene polymerization: ...

Embodiment 3

[0039] Preparation of the catalyst: Add 1.0000g (6.13mmol) of 2,6-diacetylpyridine to a 100mL Schlenk flask equipped with a stirring magnet, and inject 24.3361g (49.04) into a device equipped with a stirring magnet under the protection of argon. mmol, 8 equiv.) 2,6-dimethylaniline, 80 mL anhydrous methanol and 0.2 mL formic acid, react at 60° C. for 48 h. Cool, filter, and wash with cold methanol to obtain a yellow powdery product. After drying, it was extracted with isopropanol for 24 hours to remove the diimine by-products to obtain a pale yellow powdery intermediate. Weigh a certain amount of ligand (1.05equiv.) into a 20mL Schlenk bottle equipped with a magnetic stirrer, and add FeCl 2 ·4H 2 O(1.00equiv.). Evacuate and ventilate with argon three times, inject 10 mL of dry tetrahydrofuran under the protection of argon, and react at 25°C for 2 h. After the reaction, 5 mL of n-pentane was added, then filtered, washed with n-pentane and anhydrous ether, and dried under vacuum at r...

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Abstract

A carried metallocene catalyst or post-transition metal catalyst for the catalytic polymerization of ethylene and propylene contains Zr or Fe (0.05-1.00 wt. portions), aluminium alkylide chosen from trimethyl aluminium, triethyl aluminum and triisobutyl aluminum (1-50) and molecular sieve-like calcium silicon compound (100). Its preparing process is also disclosed. Its advantages are high catalytic activity and no adhesion to reactor.

Description

Technical field [0001] The invention relates to a supported olefin polymerization catalyst and a preparation method thereof. Background technique [0002] The metallocene catalyst and the late transition metal olefin polymerization catalyst belong to a single active center catalytic system. They not only have high catalytic activity, but also the catalyst system has the advantages of controllable polymer structure, adjustable polymer molecular weight and distribution, etc., so as to realize the molecular tailoring of polymers, which has aroused great interest of researchers (J.Am. Chem. Soc., 1995, 117: 6414 to 6415; J. Am. Chem. Soc., 1998, 120: 4049 to 4050; Chem. Commun., 1998, 849 to 850; Chem. Rev., 2000, 100: 1169). Moreover, the late transition metal catalysts have weak oxygen affinity and are beneficial to catalyze the copolymerization of polar monomers and olefins, and are expected to produce functionalized polyolefin materials with excellent performance. Therefore, meta...

Claims

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Application Information

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IPC IPC(8): C08F4/02C08F4/70C08F10/00
Inventor 胡友良郭存悦张明革马志
Owner INST OF CHEM CHINESE ACAD OF SCI
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