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Silane compound and its preparation method

A silane compound and compound technology, applied in the field of polyolefin production, can solve the problems of slow decay of catalyst activity and complicated preparation process, and achieve the effects of high isotactic index, high catalyst activity and wide molecular weight distribution

Active Publication Date: 2017-02-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Toho (Toho Titanium) Company disclosed a silane compound in its patent JP20050250579 in 2005, and found that the magnesium alcohol catalyst treated with these compounds has the characteristics of long-term catalytic activity, and the activity of the catalyst decays slowly, but the preparation process More cumbersome, it is necessary to prepare the catalyst first, and then treat it with the compound

Method used

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  • Silane compound and its preparation method
  • Silane compound and its preparation method
  • Silane compound and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0030] In a reactor (such as a reaction flask), under nitrogen protection and anhydrous conditions, add 9,9-dimethylolfluorene (5.8 g), trivinylchlorosilane (7.8 g) and tetrahydrofuran (150 mL), cool Sodium hydride (1.2 g) was added in batches within 2 hours under the same conditions, and reacted at room temperature for 4 hours after the addition was completed. Add saturated ammonium chloride aqueous solution, stir and separate the organic phase, extract three times with ether, and combine the organic phases. Wash with water and saturated sodium chloride solution successively, dry over anhydrous sodium sulfate, and remove the solvent. The residue was separated and purified by column chromatography to obtain the product 9,9-bis(trivinylsiloxymethyl)fluorene (3.8 g). 1H-NMR (δ, ppm, TMS, CDCl3): 7.25~8.17 (8H, m, ArH), 5.42~5.68 (6H, m, =CH), 5.02~5.35 (12H, m, =CH2), 4.33 ( 4H, s, OCH2).

Embodiment 2

[0032]In a reaction flask, 9,9-dimethylolfluorene (2.9 g), triethylamine (11 mL) and tetrahydrofuran (80 mL) were added under nitrogen protection and anhydrous conditions. A mixture of triallylchlorosilane (5.6 g) and tetrahydrofuran (20 mL) was added dropwise within 1 hour under cooling, and reacted at room temperature for 4 hours after the addition was complete. Heat to reflux for 6 hours. After the reaction was completed, the temperature was lowered, filtered, washed three times with ether, the organic phases were combined, dried over anhydrous sodium sulfate for 24 hours, and the solvent was removed. The residue was separated and purified by column chromatography to obtain the product 9,9-bis(triallylsiloxymethyl)fluorene (3.0 g, yield 42%). 1H-NMR (δ, ppm, TMS, CDCl 3 ): 7.20~8.16 (8H, m, ArH), 5.73 (6H, m, =CH), 5.00 (12H, m, =CH 2 ), 4.32 (4H,s,OCH 2 ), 2.04 (12H,m,CH 2 ).

Embodiment 3

[0034] In a reaction flask, under nitrogen protection and anhydrous conditions, add 2-isopropyl-2-isopentyl-1,3-propanediol (5.1 g), trivinylchlorosilane (7.8 g) and tetrahydrofuran (150 mL ), adding sodium hydride (2.4 g) in batches within 2 hours under cooling, reacting at room temperature for 4 hours after the addition, and heating to reflux for 6 hours. After the reaction was completed, it was lowered to room temperature, and saturated aqueous ammonium chloride solution was added, and the organic phase was separated after stirring. Extracted three times with ether, and combined the organic phases. Wash with water and saturated sodium chloride solution successively, dry over anhydrous sodium sulfate, and remove the solvent. The residue was separated and purified by column chromatography to obtain 2.4 g of the product 2-isopropyl-2-isopentyl-1,3-bis(trivinylsiloxy)propane. 1H-NMR (δ, ppm, TMS, CDCl 3 ):5.42~5.68(6H,m,=CH),5.02~5.35(12H,m,=CH 2 ),3.84(4H,s,OCH 2 ), 1.84(...

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Abstract

The invention discloses a silane compound and a preparation method thereof, and provides the silane compound, which can be applied to an olefin polymerization catalyst and especially applicable to being used as an internal electron donor of a propylene polymerization catalyst. The silane compound is added to the preparation process of the catalyst, so as to form a novel catalytic polymerization reaction system. Thus, the catalyst has the characteristics of high activity and orientational ability, and slow activity decay.

Description

technical field [0001] The invention relates to the technical field of polyolefin production. More specifically, the present invention relates to a catalyst for olefin polymerization and its preparation method. Background technique [0002] The active components of Ziegler-Natta catalysts for olefin polymerization or copolymerization usually contain magnesium, titanium, halogens and internal electron donors as the main components. When used in polymerization reaction, cocatalyst organoaluminum compound and external electron donor component (usually organosilane compound) should be added at the same time. Especially for the directional polymerization of propylene, when there is no external electron donor, most catalysts have low orientation, and the isotactic index of the obtained polymer is also low (generally lower than 90%), which is not conducive to Industrial applications of catalysts. Therefore, the addition of external electron donor components plays a very importan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08F10/00C08F10/06C08F4/646
Inventor 王军高明智马晶刘海涛陈建华李现忠马吉星张晓帆蔡晓霞李昌秀胡建军马长友
Owner CHINA PETROLEUM & CHEM CORP
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