A Supported Monometallocene Catalyst for Ethylene Polymerization

A single metallocene, ethylene polymerization technology, applied in the field of supported single metallocene catalyst for ethylene polymerization, can solve the problems of limited industrial application, high production cost, poor shape of carrier particles, etc., achieve high ethylene polymerization catalytic activity, Good particle shape, effect of good particle shape

Active Publication Date: 2016-09-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the homogeneous single metallocene catalyst requires a large amount of MAO to achieve high activity, the production cost is high, and the obtained polymer is amorphous, which cannot be used in the widely used slurry method or gas phase polymerization process to overcome the above problems The most effective way is to support the soluble mono-metallocene catalyst
[0003] At present, there are a lot of research reports on single metallocene loading, among which SiO 2 CN1174848; CN1174849; CN1356343; US4,808,561; US5,026,797; US5,763,543; .Appl.99 / 21898; US6,455,647; J.Mol.Catal.A2002,188,123; PCT Int.APP1.2004 / 078804; CN101817892; CN101172988; Poor and uncontrollable; although the use of spherical magnesium chloride (containing alcohol) can ensure that the catalyst loaded with a single metallocene has a good particle shape, the carrier still contains alcohol, water, alkoxy and other components, and the preparation of the carrier is complicated. The above Disadvantages limit the industrial application of MgCl-supported monometallocene catalysts
[0004] There are also literatures that use carriers containing magnesium chloride, silica gel, etc. to load mono-metallocenes (Polymer International, 200251: 417-423; US5962360), but the activity is very low, and a large amount of MAO needs to be added during polymerization

Method used

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  • A Supported Monometallocene Catalyst for Ethylene Polymerization
  • A Supported Monometallocene Catalyst for Ethylene Polymerization
  • A Supported Monometallocene Catalyst for Ethylene Polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) Preparation of chlorinated hydrocarbyl silicon / magnesium chloride support

[0052] Under the protection of nitrogen, take 5.62 grams of magnesium chloride carrier and add 100 ml of dried hexane to disperse into a suspension, add 1 ml of SiCl 2 (n-Bu) 2 , start stirring, heat up to 30° C., react for 4 hours, and dry in vacuum to obtain a solid powder with good fluidity.

[0053] (2) Preparation of alkyl aluminoxane / chlorinated hydrocarbyl silicon / magnesium chloride support

[0054] Under nitrogen protection, take 5.0 grams of the modified magnesium chloride carrier obtained above and add it to a glass reactor, add 60 milliliters of dried toluene, disperse into a suspension, and add 18 milliliters of 10 wt% MAO (methylaluminoxane) toluene solution , heated to 50 ° C, stirred for 4 hours, then washed three times with 50 ml × 3 toluene, then washed with hexane, and dried in vacuum to obtain a solid powder with good fluidity, that is, a magnesium chloride carrier conta...

Embodiment 2

[0063] (1) Preparation of chlorinated hydrocarbyl silicon / magnesium chloride support

[0064] With embodiment 1 step (1), only SiCl in embodiment 1 2 (n-Bu) 2 Change to SiCl 4 .

[0065] (2) Preparation of alkyl aluminoxane / chlorinated hydrocarbyl silicon / magnesium chloride support

[0066] Same as step (2) of Example 1.

[0067] (3) Preparation of supported metallocene catalyst B

[0068] Same as step (3) of Example 1 to obtain supported metallocene catalyst B. Characterized by ICP, in catalyst B, the weight content of Ti is 0.31%, and the weight content of Al is 11.30%.

Embodiment 3

[0070] (1) Preparation of chlorinated hydrocarbyl silicon / magnesium chloride support

[0071] With embodiment 1 step (1), only SiCl in embodiment 1 2 (n-Bu) 2 Change to CH 3 SiCl 3 .

[0072] (2) Preparation of alkyl aluminoxane / chlorinated hydrocarbyl silicon / magnesium chloride support

[0073] Same as step (2) of Example 1.

[0074] (3) Preparation of supported metallocene catalyst C

[0075] Same as step (3) of Example 1 to obtain supported metallocene catalyst C. Characterized by ICP, the weight content of Ti in catalyst C is 0.30%, and the weight content of Al is 11.18%.

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Abstract

The present invention relates to a supported monometallocene catalyst for ethylene polymerization and a preparation method thereof, the catalyst comprising (a) a monometallocene compound; (b) a chlorinated hydrocarbyl silicon modifier; (c) an alkyl aluminoxane (d) the reaction product of the magnesium chloride carrier; its preparation method includes: (1) preparation of magnesium chloride carrier modified by silicon chloride, (2) preparation of magnesium chloride carrier modified by alkyl aluminoxane, (3) magnesium chloride loaded single Preparation of metallocene catalyst; the obtained single metallocene catalyst catalyzes ethylene polymerization or copolymerization and has high polymerization activity. The preparation method of the magnesium chloride carrier used is simple, and the obtained loaded catalyst particle has good shape and adjustable size. The supported monometallocene catalyst obtained by the method catalyzes the copolymerization reaction of ethylene and α-olefin, has high copolymerization activity and the obtained resin powder has good particle shape and high packing density, and can be applied to slurry method and gas phase polymerization process .

Description

technical field [0001] The invention relates to a modified magnesium chloride supported monometallocene catalyst, a preparation method, and an application of the obtained catalyst in olefin polymerization. technical background [0002] The development and application of single metallocene catalysts is another major breakthrough in the field of olefin polymerization catalysts after the traditional Ziegler-Natta catalysts. Especially in the 1980s, Kaminsky and Sinn et al. (Angew.Chem., 1980, 19, 390; Adv Organoment.Chem., 1980, 18, 99) developed a high-efficiency cocatalyst methylaluminoxane (MAO), making the research on single metallocene catalysts enter a stage of rapid development. Because the homogeneous single metallocene catalyst requires a large amount of MAO to achieve high activity, the production cost is high, and the obtained polymer is amorphous, which cannot be used in the widely used slurry method or gas phase polymerization process to overcome the above problems...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/02C08F4/6592C08F4/02
Inventor 高榕李岩廖浩瀚周俊领刘东兵徐世媛
Owner CHINA PETROLEUM & CHEM CORP
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