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External donor compound

An external electron donor and compound technology, which is applied in the field of external electron donor compounds to achieve high stereoselectivity

Active Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the deficiency that existing external electron donor compounds cannot prepare high isotactic polymers with high catalytic activity, and provide a kind of external electron donor compound, which will contain the compound of calixarene group Used as an external electron donor compound for an olefin polymerization catalyst system, it can improve the catalytic activity, stereoselectivity and hydrogen tuning sensitivity of the olefin polymerization catalyst system, and thus can prepare high melting Index and low melt index polymers

Method used

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preparation example Construction

[0098] According to the present invention, the compound represented by formula 3 can be synthesized by conventional methods in the field of organic synthesis, without special limitation. Preferably, in the present invention, the preparation method of the calixarene compound shown in formula 3 comprises: under etherification conditions or esterification conditions, the calixarene shown in formula 6 and R 5 x 3 Contact is carried out at a molar ratio of 1:3-3.6, and the resulting product is then mixed with R 7 wxya 5 (i.e., Grignard reagent) or R 8 Li (ie, organolithium compound) is mixed at a molar ratio of 1:1-1.2 at a temperature of -70°C to 10°C, preferably at a temperature of -30°C to 10°C, and the resulting mixture is heated at 40-80°C, preferably The reaction is carried out at a temperature of 40-60°C, wherein, R 7 and R 8 Each is C 1 -C 5straight or branched chain alkyl, X 3 and x 5 Each is a halogen, such as one of chlorine, bromine and iodine, preferably chlor...

Embodiment 1

[0231] Example 1: 4-tert-butylcalix[4]arene-O, O', O"-triisobutyryl-O"'-(di-n-butylaminodiethoxy) silane (that is, in formula I, R 1 Both are ethyl, R 3 Both are n-butyl, in formula II, R 5 Both are isobutyryl, R 6 are all tert-butyl) synthesis:

[0232] (1) Preparation of 4-tert-butylcalix[4]arene

[0233] With reference to the method disclosed in p-tert-butylcalix [4] arene (p-tert-Butylcalix [4] arene) (Org.Synth, 68,324, 1990), prepare 4-tert-butyl calix [4] according to the following steps ]Aromatics:

[0234] Under nitrogen protection, in a 2500mL three-neck flask equipped with a stirring device, dropping funnel and water separator, add 100g p-tert-butylphenol, 70mL concentration is 37% by weight of formaldehyde and 1g sodium hydroxide (dissolved in 5g water) . Under the protection of nitrogen, after stirring evenly, place the three-necked flask in an oil bath, heat it to reflux, and separate the water from the water separator. After no more water is separated from ...

Embodiment 2

[0245] Example 2: 4-tert-butylcalix[4]arene-O, O', O"-triisobutyryl-O"'-(diisobutylaminodiethoxy) silane (that is, in formula I, R 1 Both are ethyl, R 3 are isobutyl, in formula II, R 5 Both are isobutyryl, R 6 are all tert-butyl) synthesis:

[0246] The title compound was synthesized by the same method as in Example 1, except that diisobutylamine was used instead of di-n-butylamine. h 1 NMR (300MHz, CDCl 3 , δ): 7.06 (6H, phenyl), 6.71 (2H, Ph), 3.83 (4H, CH 2 ), 3.80 (8H, CH 2 ), 2.68 (3H, CH), 2.52 (4H, CH 2 ), 1.67 (2H, CH), 1.35 (36H, CH 3 ), 1.20 (6H, CH 3 ), 1.09 (18H, CH 3 ), 0.9 (12H, CH 3 ).

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Abstract

The invention provides an external donor compound. Aluminium alkyl is introduced into a compound with calixarene group and organosilicon amino group; when used as an external donor compound of olefin polymerization catalyst with a main catalyst of Ziegler-Natta type catalyst, the compound can endow the olefin polymerization catalyst with high stereoselectivity and hydrogen response, so as to actively prepare a polymer with high fusion index and high isotacticity and a polymer with low fusion index and high isotacticity.

Description

technical field [0001] The present invention relates to an external electron donor compound, more specifically, relates to an external electron donor compound containing a calixarene group. Background technique [0002] Catalyst systems for the polymerization of propylene generally include a Ziegler-Natta type procatalyst, an organoaluminum cocatalyst, an internal electron donor and an external electron donor compound. [0003] Since the 1950s, polypropylene catalysts have undergone the following developments: the first generation of catalysts is TiCl 3 AlCl 3 / AlEt 2 Cl system; the second generation catalyst is TiCl 3 / AlEt 2 Cl system; the third-generation catalyst uses magnesium chloride as a carrier, benzoate as an internal electron donor, and TiCl 4 As the main catalyst, aluminum alkyl is used as the cocatalyst; the fourth generation catalyst uses phthalate as the internal electron donor, silane as the external electron donor compound, and TiCl 4 As the main catal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00C07F7/02C07F5/06C08F110/06C08F4/646C08F4/654
Inventor 李现忠马晶李昌秀高明智刘海涛王军张晓帆蔡晓霞马吉星陈建华张志会杨林娜
Owner CHINA PETROLEUM & CHEM CORP
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