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Olefin polymeric catalyst system and olefin polymerization method by using catalyst system thereof

A technology of olefin polymerization and catalyst, which is applied in the field of olefin polymerization catalyst system, can solve the problem that it is difficult to balance hydrogen adjustment sensitivity and polymer molecular weight distribution, and achieve the effect of high hydrogen adjustment sensitivity

Active Publication Date: 2013-06-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to overcome the problem that the olefin polymerization catalyst system of the existing external electron donor compound is difficult to take into account the hydrogen adjustment sensitivity and the molecular weight distribution of the polymer, and to provide a compound containing a calixarene group and a diether compound Olefin polymerization catalyst system as an external electron donor compound and an olefin polymerization method using the same, the olefin polymerization catalyst system using a diether compound and a calixarene group-containing compound as an external electron donor compound, thereby having high Hydrogen tuning sensitivity and high activity to prepare polymers with a broad molecular weight distribution

Method used

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  • Olefin polymeric catalyst system and olefin polymerization method by using catalyst system thereof
  • Olefin polymeric catalyst system and olefin polymerization method by using catalyst system thereof
  • Olefin polymeric catalyst system and olefin polymerization method by using catalyst system thereof

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preparation example Construction

[0099] 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 5 straight or branched chain alkyl, X 3 and x 5 Each is a halogen, such as one of chlorine, bromine and iodine, preferably chlo...

preparation example 1

[0156] Preparation Example 1: 4-tert-butylcalix[4]arene-O, O', O"-triisobutyryl-O"'-di-n-butylaminodiethoxysilane (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:

[0157] (1) Preparation of 4-tert-butylcalix[4]arene

[0158] 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:

[0159]Under nitrogen protection, in a 250mL three-neck flask equipped with a stirring device, dropping funnel and water separator, add 10g p-tert-butylphenol, 7mL concentration is 37% by weight of formaldehyde and 0.1g 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. ℃ temperature to continue the...

preparation example 2

[0168] Preparation 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 Both are tert-butyl) synthesis

[0169] The title compound was synthesized in the same manner as in Preparation 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 present invention provides an olefin polymeric catalyze system, the catalyst system comprises a solid component and an external electron donor compound. The solid component contains titanium, magnesium and the external electron donor compound, wherein the external electron donor compound is a silane compound containing calixarene and amino and a diether compound. The polymerization activity of the olefin polymeric catalyst is increased by comparing with exclusive use of PPDE, the hydrogen modulation susceptibility of the catalyst is substantially enhanced. The molecular weight distribution of the obtained polymer is wider than the molecular weight distribution of the polymer obtained by individually using the diether compound.

Description

technical field [0001] The present invention relates to an olefin polymerization catalyst system and an olefin polymerization process using the catalyst system. Background technique [0002] Catalysts for propylene polymerization generally include Ziegler-Natta type procatalysts, organoaluminum cocatalysts, internal electron donor compounds and external electron donor compounds. [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 compound, 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 compound, silane as the external electron donor compound, and TiCl 4 As the main catalyst, MgCl 2 As a carri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/00C08F4/649C08F4/646
Inventor 刘海涛马晶李现忠高明智李昌秀王军张晓帆马吉星蔡晓霞陈建华张志会杨林娜
Owner CHINA PETROLEUM & CHEM CORP