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Method for preparing magnesium chloride loaded late transition metal catalyst

A late-transition metal and magnesium chloride technology, which is applied in the field of preparation of magnesium chloride-supported post-transition metal catalysts, can solve problems such as uncontrollable, complicated carrier preparation, and poor particle shape of the carrier

Active Publication Date: 2010-09-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many research reports on magnesium chloride compound loaded single-site catalysts (PCT Int.Appl.99 / 21898; US6,455,647; J.Mol.Catal.A 2002,188,123; PCT Int.Appl.2004 / 078804 ), but the cost of carrier preparation and catalyst loading is high, and the particle shape of the carrier is poor and uncontrollable; although the use of spherical magnesium chloride can ensure that the supported catalyst has a good particle shape, the carrier contains alcohol, water, alkoxy and other components , the preparation of the carrier is complicated, and the above shortcomings limit the industrial application of magnesium chloride-supported single-site catalysts

Method used

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  • Method for preparing magnesium chloride loaded late transition metal catalyst
  • Method for preparing magnesium chloride loaded late transition metal catalyst
  • Method for preparing magnesium chloride loaded late transition metal catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Under nitrogen protection, in a glass reactor, add 25.21 grams of anhydrous magnesium chloride at room temperature, then add 700 milliliters of dried THF, start stirring, raise the temperature to 65 ° C, stir and dissolve for 5 hours to ensure that the magnesium chloride is completely dissolved, and then pass through Buchi B -290 spray dryer prepares spherical magnesium chloride / tetrahydrofuran particles, the content of tetrahydrofuran is 23wt%, and the particle size is D 50 is 16 microns.

[0049] Spherical magnesium chloride / tetrahydrofuran particles were vacuum-dried at 100°C for 2 hours, and then vacuum-dried at 300°C for 10 hours to obtain a spherical magnesium chloride carrier with good fluidity. No tetrahydrofuran was detected by gas chromatography analysis.

[0050] Under the protection of nitrogen, take 4.61 grams of the magnesium chloride carrier obtained above and add it to a glass reactor, add 60 milliliters of dried toluene, disperse into a suspension, add ...

Embodiment 2

[0054] Spherical MgCl / THF particles were prepared on a pilot plant.

[0055] Under the protection of nitrogen, in the reactor, add 7.2 kg of anhydrous magnesium chloride at room temperature, then add 200 liters of dried tetrahydrofuran, start stirring, raise the temperature to 65 ° C, stir and dissolve for 7 hours to ensure that the magnesium chloride is completely dissolved, and then spray through the pilot test Dryer (3 kg carrier capacity per hour) prepared spherical magnesium chloride / tetrahydrofuran particles, tetrahydrofuran content 31wt%, particle size D 50 is 26 microns.

[0056] 200 grams of spherical magnesium chloride / tetrahydrofuran particles were vacuum-dried at 100° C. for 2 hours, and then vacuum-dried at 300° C. for 10 hours to obtain a magnesium chloride carrier with good fluidity. Through gas chromatography analysis, no tetrahydrofuran was detected.

[0057] Under the protection of nitrogen, take 4.83 grams of the magnesium chloride carrier obtained above an...

Embodiment 3

[0060] Under the protection of nitrogen, take 3.74 grams of the magnesium chloride carrier obtained in Example 3 and add it to a glass reactor, add 60 milliliters of dried toluene, disperse into a suspension, add 21 milliliters of 10 wt% MAO (methylaluminoxane) toluene The solution was heated to 50° C., stirred and reacted 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 containing methylaluminoxane.

[0061] Under the protection of nitrogen, 2.25 grams of the magnesium chloride carrier containing methylaluminoxane obtained above was added to a glass reactor, and 35 milliliters of dried toluene was added to make a slurry, and 0.175 grams of Ni catalyst dissolved in 20 milliliters of toluene The solution of the precursor (2,3-bis(2,6-diisopropylphenylimine) butane nickel dibromide, see the structure below) was added dropwise into the reactor...

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Abstract

The invention discloses a method for preparing a loaded late transition metal catalyst by taking magnesium chloride as a carrier, which comprises the following steps of: (1), preparation of a magnesium chloride carrier; (2), preparation of a magnesium chloride carrier of alkyl aluminoxane; and (3), preparation of a magnesium chloride loaded late transition metal catalyst, wherein the magnesium chloride carrier is prepared by adopting a spraying method in which tetrahydrofuran is taken as a solvent. The obtained loaded late transition metal catalyst catalyzes ethylene homopolymerization or copolymerization with high polymerization activity. In the method, the preparation of the magnesium chloride carrier is simple; and the obtained loaded catalyst granule has good shape and adjustable size.

Description

technical field [0001] The invention relates to a preparation method of a late transition metal catalyst supported by magnesium chloride and an application of the obtained catalyst in olefin polymerization. Background technique [0002] During the development of olefin polymerization catalysts, the late transition metal catalysts discovered in the mid-1990s have received great development and attention. Especially Ni, Pd and Fe, Co diimine catalyst system (WO9623010, WO9827124), nickel, palladium series catalyst can generate branched even hyperbranched high molecular weight polyethylene with narrow molecular weight distribution through ethylene homopolymerization, iron, Cobalt-based catalysts produce linear polyethylene with a broad molecular weight distribution. However, olefin polymerization is carried out in a homogeneous phase, and the obtained polymer is in an amorphous state, which cannot be used in the widely used slurry method or gas phase polymerization process. ...

Claims

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Application Information

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IPC IPC(8): C08F4/80C08F4/02C08F10/00
Inventor 刘东兵王世波廖浩瀚周俊领
Owner CHINA PETROLEUM & CHEM CORP
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