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Three-activity-center composite catalyst, and method for preparing cycloolefin copolymer by using three-activity-center composite catalyst

A cycloolefin copolymer and composite catalyst technology, which is applied in the field of three active center composite catalysts, can solve the problems of poor processability and low polymerization activity of non-metallocene catalysts, and achieve the best elongation at break and impact strength, good processability, The effect of good stability

Active Publication Date: 2017-08-04
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with general metallocene ethylene-cycloolefin copolymers, the polymerization activity of this non-metallocene catalyst is relatively low, and the obtained ethylene-cycloolefin copolymers tend to obtain high molecular weight polymers, and are easy to form gels, and the processability is relatively low. Difference

Method used

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  • Three-activity-center composite catalyst, and method for preparing cycloolefin copolymer by using three-activity-center composite catalyst
  • Three-activity-center composite catalyst, and method for preparing cycloolefin copolymer by using three-activity-center composite catalyst
  • Three-activity-center composite catalyst, and method for preparing cycloolefin copolymer by using three-activity-center composite catalyst

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Experimental program
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Effect test

Embodiment 1

[0036] In a 1L tank reactor, dissolve 0.15mol of refined norbornene in 500ml of refined toluene to make a solution, add this solution to the reactor that has been flushed with nitrogen in advance, and punch ethylene (0.1MPa) several times to make the solution Saturated with ethylene, under the conditions of 60°C, 0.1MPa and stirring, add 18ml of toluene solution with a concentration of 1.72mol / L methylaluminoxane (MAO), 10μmol of salicylidene 2-mercaptoaniline titanium trichloride , 10 μmol of racemic-vinyl (diindenyl) zirconium dichloride and 10 μmol of dichlorozirconocene three-site composite catalyst, the polymerization process is supplemented by metering ethylene, and the control pressure is 0.1 MPa.

[0037] After reacting for 0.2h, stop the reaction, pour the reaction solution into ethanol (composed of 150mL hydrochloric acid and 1000mL ethanol) containing 15% (v / v%) hydrochloric acid, filter after precipitation, filter cake after washing with ethanol (300ml), and dry (d...

Embodiment 2

[0039] What used in this embodiment is a 1L tank reactor. Dissolve 0.15mol of refined norbornene in 500ml of refined toluene to make a solution, add the solution to a reactor that has been flushed with nitrogen, and punch ethylene (0.1MPa) several times to make the solution saturated with ethylene, Under the condition of 0.1MPa and stirring, add 15ml of toluene solution with a concentration of 1.72mol / L methylaluminoxane (MAO), 2μmol 3,5-di-tert-butyl salicyl 2-propylthioaniline trichloro Titanium oxide, 18 μmol racemic-vinyl (diindenyl) zirconium dichloride and 5 μmol di-n-butyl dichlorozirconocene composite catalyst with three active sites. During the polymerization process, ethylene is added by supplementary metering, and the control pressure is 0.1MPa .

[0040] After reacting for 0.5h, stop the reaction, pour the reaction solution into ethanol (composed of 150mL hydrochloric acid and 1000mL ethanol) containing 15% (v / v%) hydrochloric acid, filter after precipitation, fil...

Embodiment 3

[0042] What used in this embodiment is a 1L tank reactor. Dissolve 0.15mol of refined norbornene in 500ml of refined toluene to form a solution, add the solution to a reactor that has been flushed with nitrogen, and punch ethylene (0.1MPa) several times to make the solution saturated with ethylene. Under the condition of 0.1MPa and stirring, 1.15mmol of triethylaluminum, 21ml of toluene solution with a concentration of 1.72mol / L methylalumoxane, 18μmol of 3,5-di-tert-butylsalicyl 2-propylthio Aniline titanium trichloride, 2 μmol racemic-vinyl (diindenyl) zirconium dichloride and 15 μmol di-n-butyl dichlorozirconocene three-site composite catalyst, the polymerization process is controlled by supplementary metering of ethylene. The pressure is 0.1 MPa.

[0043] After reacting for 10h, stop the reaction, pour the reaction solution into ethanol containing 15% (v / v%) hydrochloric acid (composed of 150mL hydrochloric acid and 1000mL ethanol) and filter after precipitation, after th...

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Abstract

The invention relates to a three-activity center composite catalyst, and a method for preparing a cycloolefin copolymer by using the three-activity-center composite catalyst. Under the condition of the temperature being 40 to 95 DEG C and the pressure being 0.1 to 5.0MPa, an inert organic solvent, cycloolefin and ethylene are respectively added into a reactor; then, a chain transfer agent is added; finally, the three-activity-center composite catalyst is added for solution polymerization reaction; after the reaction is finished, the obtained reaction liquid is filtered after being precipitated; filter cake obtained through filtering is washed and dried. The method has the advantages that high catalytic activity and stable catalytic performance of the catalyst can be ensured; meanwhile, the prepared copolymer has high strength and modulus on a metallocene ethylene-cycloolefin copolymer, and has lower molecular weight and better processability relative to a non-metallocene ethylene-cycloolefin copolymer.

Description

technical field [0001] The invention relates to a composite catalyst with three active centers, in particular to a cycloolefin copolymer prepared by using the composite catalyst with three active centers, and belongs to the technical field of fine chemical industry. Background technique [0002] Cyclic-Olefin Copolymers, referred to as COC (Cyclic-Olefin Copolymers), is a class of high value-added thermoplastic engineering plastics formed by the addition and copolymerization of cycloolefins, because of its high transparency, high glass transition temperature and high chemical resistance. Attention has been paid to characteristics such as character. At present, 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. [0003] The early cycloolefin copolymerization used Ziegler-Natta catalyst, which had very low polymerization activity. W...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F210/02C08F4/6592C08F4/642
CPCC08F4/64137C08F4/65925C08F4/65927C08F232/08C08F210/02
Inventor 郭峰汪文睿李传峰任鸿平杨爱武
Owner SINOPEC YANGZI PETROCHEM
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