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Method for preparing magnesium chloride loaded non-metallocene single active site catalyst

A technology of active center and magnesium chloride is applied in the field of preparation of magnesium chloride supported non-cene single active center catalyst, can solve the problems of uncontrollable, high cost, low activity and the like, achieves high ethylene polymerization catalytic activity, good particle shape and simple preparation method Effect

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 supported metallocene catalysts (PCT Int.Appl.99 / 21898; US6,455,647; J.Mol.Catal.A2002,188,123; PCT Int.Appl.2004 / 078804), However, 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 metallocene-loaded catalyst has a good particle shape, the carrier contains a small amount of alcohol, water, alkoxy Such components have an adverse effect on the supported catalyst, and the preparation of the carrier is complicated. The above shortcomings limit the industrial application of magnesium chloride-supported metallocene catalysts.
[0004] There are also literatures that use carriers containing magnesium chloride, silica gel, etc. to load metallocenes (Polymer International, 51: 417-423, 2002; 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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  • Method for preparing magnesium chloride loaded non-metallocene single active site catalyst
  • Method for preparing magnesium chloride loaded non-metallocene single active site catalyst
  • Method for preparing magnesium chloride loaded non-metallocene single active site catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0045] 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.

[0046] 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.

[0047] Under nitrogen protection, take 4.72 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 28 mill...

Embodiment 2

[0051] Spherical MgCl / THF particles were prepared on a pilot plant.

[0052] 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.

[0053] 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.

[0054] Under the protection of nitrogen, take 4.63 grams of the magnesium chloride carrier obtained above an...

Embodiment 3

[0057] Under the protection of nitrogen, take 3.62 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.

[0058] 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 0.195 grams (L2 ) 3 Zr 2 Cl 4 (Its structure is as follows, see Chinese patent application 200410086388.8 for synthesis) solution was added dropwise into the reactor, reacted at 30°C for 30 minutes, then washed with...

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Abstract

The invention discloses a method for preparing a loaded non-metallocene single active site 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 non-metallocene single active site catalyst, wherein the magnesium chloride carrier is prepared by adopting a spraying method in which tetrahydrofuran is taken as a solvent. The obtained loaded non-metallocene single active site catalyst catalyzes ethylene polymerization 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 magnesium chloride-supported non-hydrocene single active center catalyst and the application of the obtained catalyst in olefin polymerization. Background technique [0002] In the development of olefin polymerization catalysts, the non-cene catalysts developed in the 1990s have received great development and attention. In particular, the Group IV transition metal complexes (EP 0874005, WO 0155231) containing phenoxy-imine ligands have high catalytic olefin polymerization activity, and can obtain functionalized polyolefin resins with good application prospects. 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. [0003] At present, there are a lot of research reports on the support of single-site catalysts, among which SiO 2 It is reported t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/76C08F4/02C08F10/00
Inventor 刘东兵周俊领廖浩瀚刘克黄廷杰王丽莎
Owner CHINA PETROLEUM & CHEM CORP
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