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Olefin polymerization supported metallocene catalyst and preparation method thereof

A technology for metallocene catalysts and olefin polymerization, applied in the field of supported metallocene catalysts and their preparation, can solve the problems of low utilization rate of metallocene compounds, reduction of active centers, multiple prices, etc., and achieve activity maintenance, reduced dosage, and uniform distribution Effect

Active Publication Date: 2014-06-04
PETROCHINA CO LTD
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it was found in the experiment that during the process of loading the metallocene compound and alkylaluminoxane on the carrier, due to the high local concentration of the metallocene active center at the initial stage of the reaction, when combined with the cocatalyst, the effective active center decreased, making the metallocene The compound utilization rate is low. In the process of preparing metallocene catalysts, it is usually necessary to use more metallocene compounds and expensive alkylaluminoxane cocatalysts

Method used

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  • Olefin polymerization supported metallocene catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of alkylammonium methylated polystyrene chlorides: the same preparation method was used in Examples 1-3 to obtain trimethylammonium methylated polystyrene chlorides with different molar contents of ammonium functional groups.

[0025] In a 500ml round bottom flask, add 10g of chloromethylated polystyrene resin containing 8% divinylbenzene (chloromethyl molar content is 12%), add 120ml trimethylammonium, and react at room temperature for 4 hours, The solid obtained after filtration was vacuum-dried at 110° C. for 12 hours to obtain 10.6 g of trimethylammonium methylated polystyrene chloride, and the molar content of ammonium groups was 11.6%.

[0026] 21.0 grams of Davison955 silica carrier from Grace Company (specific surface area 300 m2 / g, pore volume 1.58 ml / g, average particle size 46 μm) was placed in a muffle furnace and calcined at 600° C. for 6 hours under nitrogen protection. Add the treated silica to a 500ml nitrogen-substituted reactor, add 90ml of...

Embodiment 2

[0028] 21.0 g of Davison955 silica carrier from Grace Company was placed in a muffle furnace and calcined at 600° C. for 6 hours under the protection of nitrogen. Add the treated silica to a 500ml nitrogen-substituted reactor, add 90ml of 10% (mass percent) methylalumoxane (produced by PetroChina Lanzhou Chemical Research Center) in toluene, and stir at 20°C for 1 hour. In another 250ml flask, add 0.56g (n-BuCp) 2 ZrCl 2 (bis-n-butylcyclopentadienyl zirconium dichloride) metallocene compound, 80ml toluene and 1.9 grams of trimethylammonium methylated polystyrene chloride (ammonium molar content is 11.6%, 8% DVB), stirred for 1 Hour. Add the metallocene compound reaction liquid to the silica slurry treated with methylaluminoxane, keep the temperature of the reactor at 20°C, stir for 0.5 hours, then react at -20°C for 3 hours, remove the solvent after the reaction, After drying, a pale yellow free-flowing powder was obtained, designated as cat2. The aluminum content is 13.2%...

Embodiment 3

[0030] 19.8 grams of Davison955 silica carrier from Grace Company was calcined in a muffle furnace at 600° C. for 6 hours under the protection of nitrogen. The treated silicon dioxide was added to a 500 ml reactor replaced with nitrogen, 105 ml of 10% (mass percent) methylaluminoxane toluene solution was added, and stirred at 20° C. for 1 hour. In another 250ml flask, add 0.61 g (n-BuCp) 2 ZrCl 2 (bis-n-butylcyclopentadienyl zirconium dichloride) metallocene compound, 80ml toluene and 1.9 grams of trimethylammonium methylated polystyrene chloride (ammonium molar content is 11.6%, 8% DVB), stirred for 1 Hour. Add the metallocene compound reaction liquid to the silica slurry treated with methylaluminoxane, keep the temperature of the reactor at 20°C, stir for 0.5 hours, then react at -20°C for 3 hours, remove the solvent after the reaction, After drying, a pale yellow free-flowing powder was obtained, designated as cat3. The aluminum content is 14.4% by weight and the zircon...

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Abstract

The invention relates to an olefin polymerization supported metallocene catalyst and a preparation method thereof. The olefin polymerization supported metallocene catalyst mainly comprises an inorganic silica silica-gel carrier, alkylammonium methyl polystyrene chloride, a metallocene and a metallocene cocatalyst. The alkylammonium methyl polystyrene chloride serving as a sustained release agent is reacted with the metallocene to immobilize the metallocene in a skeleton network, and the metallocene is released in the supporting process and is supported by a carrier activated by alkyl aluminoxane, so that metallocene active centers are distributed uniformly, and a condition that effective active centers are reduced after the metallocene is combined with the cocatalyst because the local concentration of the metallocene active centers is too high is avoided. Therefore, by the method, the utilization efficiency of the metallocene in high price is improved, the production cost of the metallocene catalyst is reduced and the activity of the catalyst is kept.

Description

technical field [0001] The invention relates to a metallocene catalyst and a preparation method thereof, in particular to a supported metallocene catalyst and a preparation method thereof. technical background [0002] When the metallocene catalyst is applied industrially, it is generally necessary to support the metallocene / alkylaluminoxane homogeneous catalyst system. At present, there are many reports on metallocene catalysts. US4,808,561, US5,026,797, US5,763,543, US5,661,098, US6,455,647, CN1174549, CN1356343 reported the preparation of supported metallocene catalysts with inorganic substances such as silica, magnesium chloride, alumina and the like as carriers. Although the supported metallocene catalyst prepared above does not need to use a large amount of alkylaluminoxane as a cocatalyst, due to the low activity of the catalyst, there are more catalyst residues in the polymer, which causes problems in polymer processing and makes The quality of the polymer deterior...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/00C08F10/02C08F4/6592C08F4/02
Inventor 王雄姚培洪朱博超徐人威韦少义贾军纪杨世元张鹏任峰葛汉青刘文霞张翠玲巨娟霞高冬梅王海张平生
Owner PETROCHINA CO LTD
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