Process for synthesizing supported post-transition metal catalyst

A technology of a late transition metal and a synthesis method, which is applied in the field of synthesis of supported catalysts, and achieves the effects of simplifying the preparation process, reducing the cost, and improving the catalytic performance of olefins

Inactive Publication Date: 2005-08-17
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few reports on the support of late transition metal olefin catalysts. Ma Zhi et al. 2 Supported late transition metal complexes / triethylaluminum catalyzed ethylene polymerization have been studied ("Molecular Catalysis" 2001, Vol.15, No.6); KR2000016716 discloses that late transition metal compounds are supported on silica gel for gas phase polymerization process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Add 0.5 g of 2,6-diacetylpyridine and 30 mL of solvent methylene chloride into a 100 mL round-bottomed flask, and then accurately add 2,4 times (moles) the amount of 2,6-diacetylpyridine under stirring, 4-Dimethylbenzimine, add 5 drops of formic acid (A.R) dropwise. Heat up to 50°C, reflux for 48 hours, then spin dry the solvent with a rotary evaporator to obtain a wine-red oil, add 20 mL of frozen anhydrous methanol, filter after precipitation of yellow-green powder, and wash repeatedly with frozen anhydrous methanol, The obtained yellow-green powder is vacuum-dried to obtain the ligand.

[0019] 2) The system was vacuum pumped three times with argon, and the ligand and equimolar FeCl 2 .4H 2 O was added to the two-necked flask, dichloromethane solvent was added, and the reaction was carried out at 80°C for 1.5 hours. When the temperature was lowered to 0°C, 5 times (mole) of FeCl 2 .4H 2 A solution of 3 mol / L of trimethylaluminum O (the solvent is n-hexane), re...

Embodiment 2

[0024] 1) The ligand is prepared by the same method as in Example 1.

[0025] 2) The system was vacuumed three times with argon, and the ligand and equimolar CoCl 2 .6H 2 O was added to the two-necked flask, dichloromethane solvent was added, and the reaction was carried out at 80°C for 2 hours. When the temperature was lowered to -5°C, 6 times (mol) of CoCl 2 .6H 2 3 mol / L solution of trimethylaluminum O (solvent is toluene), reacted for 8 hours, finally added 3 grams of silica gel, refluxed at 80° C. for 3 hours, and obtained the catalyst product by draining the solvent. Used for ethylene slurry polymerization (polymerization temperature 80°C, polymerization pressure 0.012MPa), polymerization activity is 3.38×10 6 gPE / molFe.h.atm.

Embodiment 3

[0027] 1) The ligand is prepared with 2,6-diacetylpyridine and 2-ethylbenimine, and the preparation process is the same as in Example 1.

[0028] 2) The system was vacuum pumped three times with argon, and the ligand and equimolar FeCl 2 .4H 2 O was added to the two-necked flask, dichloromethane solvent was added, and the reaction was stirred for 3 hours at 60°C. When the temperature was lowered to 0°C, 5 times (mol) of FeCl was added under stirring. 2 .4H 2 3 mol / L solution of trimethylaluminum O (solvent is toluene), continued to react for 6 hours, then added 3 grams of silica gel, refluxed at 80° C. for 3 hours, and obtained the catalyst product through draining the solvent. Used for ethylene slurry polymerization (polymerization temperature 80°C, polymerization pressure 0.012MPa), polymerization activity is 3.28×10 6 gPE / molFe.h.atm

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Abstract

The invention provides a process for synthesizing load type post-transition metallic catalyst, wherein crystallinic water of aqueous metal salt is used during the preparation of three coordination Fe, Co complex by double imines pyridine ligand, thus making the added alkyl aluminium directly synthesize alkyl aluminium oxygenalkyl and load it onto carrying agent, thus realizing the one step preparation for load type post-transition metallic catalyst.

Description

technical field [0001] The invention relates to a method for synthesizing a supported catalyst, in particular to a method for synthesizing a supported late transition metal catalyst, especially an iron-based late transition metal catalyst. Background technique [0002] Late transition metal catalysts are a more novel class of olefin polymerization catalysts than metallocene catalysts. It maintains many advantages of metallocene catalysts, and can adjust and control the structure, molecular weight and branching degree of polymers, so as to produce special resins suitable for special occasions and excellent performance according to requirements, making up for Ziegler-Natta catalysts. deficiencies in this area. In addition, compared with metallocene catalysts, the synthesis of late transition metal catalysts is relatively simple and the yield is higher; the amount of cocatalyst used in polymerization is equivalent to that of supported metallocene catalysts, so its cost is much...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/02C08F4/602
Inventor 贾军纪朱博超陈雪蓉赵晓东魏红李林青韦少义徐晓敏王德平姚培洪
Owner PETROCHINA CO LTD
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