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Method for preparing copolymer of ethylene and/or alpha-olefin and cycloolefin and catalysis system thereof

A technology of cycloolefin copolymer and catalytic system, which is applied in the field of preparing ethylene and/or α-olefin and cycloolefin copolymer, can solve the problems of increasing the cost of the post-processing process, unfavorable industrialization development, increasing the content of metals, etc., to achieve Reduce catalyst and co-catalyst residues, facilitate subsequent treatment, and reduce dosage

Active Publication Date: 2018-11-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The metallocene catalyst is used as the main catalyst, and the alkylaluminoxane is used as the cocatalyst to carry out solution polymerization to produce COC. Although the activity is relatively high, due to the expensive cocatalysts MAO (methyl aluminoxane), MMAO (modified methyl aluminum Oxane) or dMAO (dry methyl aluminoxane) in large quantities use greatly increases production cost, also increases the content of the metal in the polymer greatly simultaneously, increases the cost of aftertreatment process, is unfavorable for its industrialization develop

Method used

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  • Method for preparing copolymer of ethylene and/or alpha-olefin and cycloolefin and catalysis system thereof
  • Method for preparing copolymer of ethylene and/or alpha-olefin and cycloolefin and catalysis system thereof
  • Method for preparing copolymer of ethylene and/or alpha-olefin and cycloolefin and catalysis system thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] What used in this embodiment is a 1L tank reactor. First 36.880mg (4 × 10 -5 mol) Ph 3 CB(C 6 f 5 ) 4 Dissolve in 10mL toluene to make a concentration of 4×10 -3 mol / L solution, stand-by; 8.37mg rac-[Et(Ind) 2 ]ZrCl 2 (2×10 - 5mol) was dissolved in 8.37mL of toluene to form a solution for use. Dissolve 265.770g (2.827mol) norbornene in a certain amount of toluene to prepare 476.16mL norbornene toluene solution. The solution was added to the reactor previously flushed with nitrogen, and the ethylene (5bar) was punched several times to make the solution saturated with ethylene. The initial molar ratio of ethylene is 14.0), followed by adding 5.48mL triisobutylaluminum toluene solution with a concentration of 1.1mol / L, 10mL Ph 3 CB(C 6 f 5 ) 4 Toluene solution, 8.37mL catalyst solution, start polymerization; during the polymerization process, the pressure is controlled at 5 bar by supplementing ethylene.

[0038] After 30 minutes of reaction, the reaction so...

Embodiment 2

[0040] What used in this embodiment is a 100mL tank reactor. First mix 30mL toluene and 30mL cyclohexane to make a mixed solvent for use; 3.688mg (4×10 -6 mol) Ph 3 CB(C 6 f 5 ) 4 Dissolve in 1mL of mixed solvent of toluene and cyclohexane to make a concentration of 4×10 -3 mol / L solution, ready for use; 0.84mg rac-[Et(Ind) 2 ]ZrCl 2 (2×10 -6 mol) was dissolved in 0.84mL mixed solvent to form a solution, ready for use. Dissolve 26.577g (0.282mol) norbornene in a certain amount of mixed solvent to prepare 47.61mL norbornene solution. This solution is added in the reactor that has flushed with nitrogen in advance, punches ethylene (5bar) repeatedly, makes solution be saturated by ethylene, under the condition of 50 ℃ of temperature, 5bar and stirring (600r / min) (norbornene and The initial molar ratio of ethylene is 12.4), followed by adding 0.55 mL of triisobutylaluminum cyclohexane solution with a concentration of 1.1 mol / L, 1 mL Ph 3 CB(C 6 f 5 ) 4 Solution, 0.84m...

Embodiment 3

[0043] What used in this embodiment is a 100mL tank reactor. First 3.690mg (4 × 10 -6 mol) Ph 3 CB(C 6 f 5 ) 4 Dissolve in 1mL toluene to make a concentration of 4×10 -3 mol / L solution, ready for use; 0.84mg rac-[Et(Ind) 2 ]ZrCl 2 (2×10 - 6 mol) was dissolved in 0.84mL toluene to form a solution, ready for use. Dissolve 13.289g (0.141mol) of norbornene and 16.920g (0.141mol) of ethylidene norbornene in a certain amount of toluene to prepare 47.61mL of norbornene toluene solution. This solution is added in the reactor that has flushed with nitrogen in advance, punches ethylene (5bar) several times, makes solution saturated by ethylene, under the condition of 60 ℃ of temperature, 5bar and stirring (600r / min) (norbornene, The initial molar ratio of ethylidene norbornene to ethylene is 7.0:7.0:1), followed by adding 0.55mL triisobutylaluminum toluene solution with a concentration of 1.1mol / L, 1mL Ph 3 CB(C 6 f 5 ) 4 Toluene solution and 0.84mL catalyst solution were ...

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Abstract

The invention discloses a catalysis system for preparing a copolymer of ethylene and / or alpha-olefin and cycloolefin. The catalysis system comprises a main catalyst and cocatalysts. The main catalystis a metallocene compound. The cocatalysts comprise an organoboron compound and alkyl aluminum. The invention also discloses a method for preparing the copolymer of ethylene and / or alpha-olefin and cycloolefin through the catalysis system. The method comprises that an inert organic solvent, ethylene and / or alpha-olefin and cycloolefin are sequentially added in a reactor at a temperature of 40 to 100 DEG C under pressure of 1 to 30 bar, after the ethylene and / or alpha-olefin is dissolved in the inert organic solvent until saturation, a triisobutyl aluminum solution, a metallocene catalyst solution and an organoboron compound solution are orderly added into the solution and the mixed solution undergoes a reaction. Compared with MAO, MMAO, and dMAO, the cocatalysts can efficiently polymerizethe cycloolefin copolymer, the metal content of the polymerization product is reduced and the post-treatment cost is greatly reduced.

Description

technical field [0001] The present invention relates to a method for preparing ethylene and / or alpha-olefin and cycloolefin copolymer and the catalyst system used. Background technique [0002] Cyclic-Olefin Copolymers, referred to as COC (Cyclic-Olefin Copolymers), are a class of high value-added thermoplastic engineering plastics that are copolymerized from cyclic olefins. Due to its high transparency, extremely low dielectric constant, excellent moisture barrier, heat resistance, chemical stability and dimensional stability, it has been widely used in the manufacture of various optical lenses, automotive headlights, LCD Components, electronic and electrical components, pharmaceutical and food packaging materials, etc. In addition, COC is also considered to be the best material to replace PC for the production of next-generation high-density DVD. [0003] The early cycloolefin copolymerization used Ziegler-Natta catalyst, which had very low polymerization activity. With ...

Claims

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Application Information

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IPC IPC(8): C08F232/08C08F210/02C08F210/06C08F210/14C08F4/6592
CPCC08F232/08C08F210/02C08F210/14C08F210/06C08F4/65925
Inventor 曹堃夏天姚臻马达锋
Owner ZHEJIANG UNIV
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