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Bridge non-metallocene and preparation and application thereof

A non-metallocene, bridge-type technology, applied in the field of non-metallocene catalysts for olefin polymerization and olefin polymerization, can solve the problems of high cost, difficult structure modification, poor stability, etc., and achieve high insertion rate, high molecular weight, and good stability Effect

Active Publication Date: 2013-12-11
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The discovery of metallocene catalysts has led to a great progress in olefin catalysts, but due to a series of limiting factors in metallocene catalysts, such as poor stability, high cost, and difficulty in structural modification, the research direction of olefin catalysts has shifted to possible Non-metallocene catalysts that change ligand structure (1. Xi Xiaoli. Research progress of non-metallocene catalysts[J]. Petrochemical Technology and Application, 2002, 20, 327-333. 2. Liu Weijiao, Huang Qigu, Yi Jianjun, etc. Olefin Coordination Polymerization Research progress of catalysts [J]. Polymer Bulletin, 2010, 6, 1-33.)

Method used

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  • Bridge non-metallocene and preparation and application thereof
  • Bridge non-metallocene and preparation and application thereof
  • Bridge non-metallocene and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1) Preparation of sodium salicylaldehyde phenate: under the protection of high-purity nitrogen, add 0.38g (9.5mmol) sodium hydroxide and 60mL absolute ethanol to a 300mL reaction flask, and stir to completely dissolve the sodium hydroxide in absolute ethanol . In this solution, add 1mL salicylaldehyde dropwise, react at room temperature for 3h, let stand, filter, wash 2-3 times with absolute ethanol, get 1.31g pale yellow powdered sodium salicylaldehyde phenate after draining, the yield 91.3%.

[0047] 2) Preparation of Schiff base sodium phenate: in a 300mL reaction bottle filled with high-purity nitrogen atmosphere, disperse 0.72g sodium salicylaldehyde phenate (5mmol) solid with absolute ethanol, stir, add 0.62g (5mmol) 2- Amino-4-methylphenol. At 80°C, reflux for 8h. Cool, let stand, filter, wash, and drain to obtain 0.65 g of red solid powder of Schiff base sodium phenolate, with a yield of 73.5%.

[0048] 3) Ligand preparation: Anhydrous and oxygen-free and un...

Embodiment 2

[0052] 1) Preparation of Schiff base sodium phenate: In a 300mL reaction flask filled with a high-purity nitrogen atmosphere, disperse 0.72g of sodium salicylaldehyde phenate (5mmol) solid with absolute ethanol, stir, and add 0.62g (5mmol) of 2- Amino-5-methylphenol. At 80°C, reflux for 8h. Cool, let stand, filter, wash, and drain to obtain 0.63 g of red solid powder of Schiff base sodium phenolate, with a yield of 71.8%.

[0053] 2) Preparation of the ligand: Anhydrous and oxygen-free and under the protection of high-purity nitrogen, take 0.55g of Schiff base sodium phenolate, disperse it in 30ml of toluene, and add 0.36ml (2mmol) of diphenyl to it dropwise at 0°C Phosphorus chloride was reacted for 2 hours, allowed to stand, filtered, washed, recrystallized, and vacuum-dried to obtain 0.46 g of ligand L2 with a yield of 33.5%.

[0054] 3) Preparation of non-metallocene main catalyst for olefin polymerization: under the protection of nitrogen atmosphere, take 0.20 g (0.8 mm...

Embodiment 3

[0057] 1) Preparation of Schiff base sodium phenate: In a 300mL reaction flask filled with high-purity nitrogen atmosphere, disperse 0.72g sodium salicylaldehyde phenate (5mmol) solid with absolute ethanol, stir, add 0.83g (5mmol) 2- Amino-4-tert-butylphenol. At 80°C, reflux for 8h. Cool, let stand, filter, wash, and drain to obtain 0.91 g of red solid powder, with a yield of 62.1%.

[0058] 2) Ligand preparation: Anhydrous and oxygen-free and under the protection of high-purity nitrogen, take 0.58g of Schiff base sodium phenolate, disperse it in 30ml of toluene, and add 0.36ml (2mmol) of diphenyl to it dropwise at 0°C Phosphorous chloride was reacted for 2 hours, allowed to stand, filtered, washed, recrystallized, and vacuum-dried to obtain 0.27 g of ligand L3, with a yield of 30.1%.

[0059] 3) Preparation of non-metallocene procatalyst for olefin polymerization: Under the protection of nitrogen atmosphere, 0.18g (0.4mmol) of ligand L3 was taken and dissolved in 30ml of to...

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Abstract

The invention relates to a bridge non-metallocene and preparation and application thereof. The structure of the bridge non-metallocene is shown in a general formula (1), wherein in the general formula (1), M is Ti, Zr, Ni, Nd, Y, Rh, Hf, Sc, La or Sm; X is Cl or Br; R is H, C1-C10 aliphatic groups, and C6-C20 arene groups; and R'1, R'2, R'3, R'4, R1, R2, R3 and R4 are H or C1-C10 aliphatic groups, wherein any two substituents can be the same or different. The bridge non-metallocene is used for catalyzing non-polar olefin polymerization or copolymerization, or non-polar olefin and polar olefin copolymerization; and the bridge non-metallocene is high in catalytic activity, good in stability and less in application amount of a catalyst promoter, the molecular weight of an obtained copolymer is high, and an insertion rate of monomers is high.

Description

technical field [0001] The invention belongs to the fields of non-metallocene catalysts for olefin polymerization and olefin polymerization, and specifically relates to the preparation of bridge-type non-metallocene catalysts for ethylene polymerization or olefin copolymerization and the preparation of olefin polymers. Background technique [0002] The development of the polyolefin industry depends on the research and development of catalysts. Looking at the development of catalysts, from the initial Ziegler-Natta catalysts to today's non-catalyst catalysts, the polyolefin industry has also been rapidly developed and widely used. prospect. The discovery of metallocene catalysts has led to a great progress in olefin catalysts, but due to a series of limiting factors in metallocene catalysts, such as poor stability, high cost, and difficulty in structural modification, the research direction of olefin catalysts has shifted to possible Non-metallocene catalysts that change lig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/46C08F4/642C08F4/70C08F4/52C08F10/00C08F10/02C08F10/06
Inventor 义建军胡徐腾黄启谷朱百春毛静李红明袁苑孙天旭张明革张新莉甄鸿鹏王仪森
Owner PETROCHINA CO LTD
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