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Boroxol titanocene metal catalyzer and preparation method and application thereof

A technology of titanocene catalyst and boron oxygen, which is applied in the field of boroxy titanocene catalyst and its preparation, can solve the problems of poor solubility and difficulty, and achieve the effects of simple method, guaranteed catalytic efficiency, increased solubility and stability

Active Publication Date: 2010-06-02
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN1065870C, CN1065871C ​​and CN1340551A provide a kind of synthetic method of oxygen-containing titanocene, the synthesized catalyst has good activity to the syndiotactic polymerization of styrene; CN1345887A and CN1593763A provide a kind of synthetic method of oxygen-containing titanocene, so The synthesized catalyst has good activity for the polymerization of ethylene or ethylene and propylene; the above-mentioned catalysts generally introduce oxygen atoms into the catalyst molecule through alkoxy and phenoxy groups to stabilize the molecular structure of the catalyst, and finally compound with aluminoxane , to form an efficient catalytic system for olefin polymerization; the above-mentioned catalysts generally have poor solubility in hexane, and are not easily used in homogeneous or slurry polymerization using hexane as a solvent

Method used

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  • Boroxol titanocene metal catalyzer and preparation method and application thereof
  • Boroxol titanocene metal catalyzer and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of diisooctyl borate titanium trichloride.

[0019] Add 50 milliliters of hexane, 1.90 grams of TiCl 4 (10 mmol) to 0.025M 3 Nitrogen gas was introduced at the flow rate of / h, and 2.86 g of di-isooctyl borate (10 mmol was diluted with 20 ml of hexane) was added dropwise at a constant speed within 20 minutes, and reacted for 2 hours to generate a red solution. Evaporation of the solvent gave 4.38 g of a reddish-brown liquid. Molecular formula C 16 h 34 BO 3 Cl 3 Ti, the molecular weight is 439.23. Elemental analysis: C (wt%), measured value (theoretical value): 43.70 (43.71); H (wt%), measured value (theoretical value): 7.75 (7.74); chemical analysis: Cl (wt%), measured value (Theoretical value): 24.28 (24.25).

Embodiment 2

[0021] Preparation of diisooctyl borate titanocene dichloride.

[0022] Add 50 milliliters of hexane, 0.2134 grams of 1,2,3,4-tetramethyl-5-trimethylsilyl-cyclopentadiene into a stirred reaction flask of 100 milliliters after anhydrous and oxygen-free treatment, and stir 0.4392 g of diisooctyl borate titanium trichloride (1 mmol) was added dropwise at room temperature, and after the dropwise addition was completed, it was reacted at 65° C. for 24 hours to form a red solution. The precipitate was filtered off, and the solvent was evaporated to obtain 0.5048 g of a reddish-brown liquid. Molecular formula C 25 h 47 BO 3 Cl 2 Ti, the molecular weight is 525. Elemental analysis: C (wt%), measured value (theoretical value): 57.18 (57.14); H (wt%), measured value (theoretical value): 8.96 (8.95); chemical analysis: Cl (wt%), measured value (Theoretical value): 13.53 (13.52).

Embodiment 3

[0024] Preparation of Diisooctyl Dichloromonoindene Titanium Borate.

[0025] Add 50 ml of hexane, 0.2068 g of 5-trimethylsilyl-indene (1.1 mmol) hexane to a 100 ml stirred reaction flask that has been treated with anhydrous and anaerobic treatment, to suspend the turbid and turbid liquid, and drop it at room temperature under stirring. Add 0.4754 g diisooctyl borate titanium trichloride (1 mmol), and react at 65° C. for 24 hours after the dropwise addition to form a red solution. The precipitate was filtered off, and the solvent was evaporated to obtain 0.4302 g of a reddish-brown liquid with a yield of 77.5%. Molecular formula C 25 h 41 BO 3 Cl 2 Ti, the molecular weight is 519. Elemental analysis: C (wt%), measured value (theoretical value): 57.83 (57.81); H (wt%), measured value (theoretical value): 7.89 (7.90); chemical analysis: Cl (wt%), measured value (Theoretical value): 13.70 (13.68).

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Abstract

The invention relates to a boroxol monotitanocene catalyst with high polymerization activity to alpha-olefin and high solubility in water, a relative preparation method and an application. The preparation method comprises synthesizing borate titanium trichloride from borate and titanium tetrachloride at the mol ratio of 1.00-1.05, reacting trimethylsilyl compound of cyclopentadienyl, lindenyl or relative derivative with borate titanium trichloride at the mol ratio of 1.05-1.10 to obtain borate titanium trichloride, reacting phenol or alcohol, pyrindine and borate dichloro monotitanocene at themol ratio of 1:1:1.05-1:1:1.1 to obtain boroxol monotitanocene catalyst. The invention uses borate group to lead into oxygen atoms, thereby stabilizing molecule structure and improving the solubilityand stability of the product in hexane with confirmed catalysis efficiency. The product is suitable for the homogeneous or slurry polymerization whose solvent is hexane. The synthesis method is simple. And the product can be used to synthesize the homopolymer or copolymer from ethylene or / and alpha olefin.

Description

technical field [0001] The invention relates to a boroxy-mono-titanocene catalyst containing boron-oxyl ligands, which is easily soluble in hexane and has high polymerization activity for α-olefins, as well as its preparation method and application. Background technique [0002] The development of highly active olefin polymerization catalysts has always been the focus of researchers' work. In recent years, the synthesis and development of monocene ligand catalysts have been paid more and more attention. CN1065870C, CN1065871C ​​and CN1340551A provide a kind of synthetic method of oxygen-containing titanocene, the synthesized catalyst has good activity to the syndiotactic polymerization of styrene; CN1345887A and CN1593763A provide a kind of synthetic method of oxygen-containing titanocene, so The synthesized catalyst has good activity for the polymerization of ethylene or ethylene and propylene; the above-mentioned catalysts generally introduce oxygen atoms into the catalyst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/6592C08F10/00
Inventor 张红江蔡小平王笑海东升魁陈可佳金春玉陶青海刘洪伟
Owner PETROCHINA CO LTD
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