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Polymeric catalyst system of norbornaene and its preparing process

A technology of norbornene and polymerization catalysis, applied to the use of the above-mentioned catalytic system in the polymerization of norbornene and its derivatives, the preparation of the above-mentioned catalytic system, [2--4 fields, can solve the waste of norbornene resources, etc. problems, to achieve the effects of stable performance, simple preparation and easy availability of raw materials

Inactive Publication Date: 2003-01-15
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The petrochemical industry produces a large amount of norbornene by-products every year, but because there is no good catalyst in our country to convert it into norbornene polymer, most of the norbornene resources are wasted

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1.N, the preparation of O bidentate ligand: with 30 milliliters of glacial acetic acid, 8.8 millimoles (mmol) of 3-tert-butyl-2-hydroxybenzaldehyde and 8.6 millimoles (mmol) of diphenyl ketone and The ammonium acetate of 64 millimoles (mmol) is placed in 250 milliliters (mL) round-bottomed flask, after stirring and refluxing for 4 hours, this mixed solution is cooled to room temperature, pours in 500 milliliters of saturated sodium bicarbonate solutions under stirring then, obtains white solid. After filtration, the white solid was dissolved in 50 ml of dichloromethane, diffused therein with n-pentane, and white crystals were precipitated, with a yield of 85%. Elemental analysis measured values: C, 81.51; H, 6.55; N, 7.56; O, 4.38%; C 25 h 24 N 2 Theoretical value of O: C, 81.49; H, 6.57; N, 7.60; O, 4.34%; 1 H NMR (CDCl 3 ): 1.49(s, 9H), 5.31(s, 1H), 6.85-7.83(m, 13H), 10.02(s, 1H);

[0030] 2. Preparation of catalyst:

[0031] Dissolve 2 mmoles of the white pro...

Embodiment 2

[0034] 1, the preparation of catalyst: preparation method is with embodiment one.

[0035] 2. Norbornene polymerization: Vacuumize the dry 250 ml Schlenk bottle with a stirring magnet, and replace it with nitrogen for three times, so that the reaction system is in a nitrogen environment, add 5 μmol of the catalyst prepared in step 1, 20 ml Toluene, then add 1.00 gram of norbornene (norbornene monomer and catalyst molar ratio is 2100), after stirring for 5 minutes at 25 ℃, add 5.4 milliliters of procatalyst MAO (MAO / catalyst molar ratio is 1500), at 25 After reacting for 60 minutes at ℃, add 5ml of isobutanol to terminate the polymerization, then add 100 milliliters of 5‰ hydrochloric acid ethanol (volume ratio), stir at room temperature for 10 hours, then leave to stand for 2 hours and filter, and the obtained polymer Vacuum drying for 40 hours gave 0.3480 grams of polymer, a conversion rate of 34.8%, and a catalyst activity of 7.0×10 4 gPNB / (molNi h atm). Polymer weight ave...

Embodiment 3

[0037] 1, the preparation of catalyst: preparation method is with embodiment one.

[0038] 2. Norbornene polymerization: Vacuumize the dry 250 ml Schlenk bottle with a stirring magnet, and replace it with nitrogen for three times, so that the reaction system is in a nitrogen environment, and add 5 micromoles (μmol) prepared in step 1. 20 milliliters of toluene, then add 1.00 grams of norbornene (norbornene monomer and catalyst molar ratio is 2100), after stirring for 5 minutes at 25 ℃, add 7.2 milliliters of procatalyst MAO (MAO / catalyst molar ratio is 2000), after reacting for 60 minutes at 25°C, add 5ml isobutanol to terminate the polymerization, then add 100 milliliters of 5‰ hydrochloric acid ethanol (volume ratio), stir at room temperature for 10 hours, then leave to stand for 2 hours and filter to obtain The polymer was vacuum-dried at 80° C. for 40 hours to obtain 0.5602 grams of polymer, the conversion rate was 56.02%, and the catalyst activity was 1.1×10 5 gPNB / (molN...

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Abstract

A catalyst system for polymerizing norbornaene is composed of the primary catalyst, [2-(2'-substituent-hydroxyphenyl)-4,5-diphenyl imidazole]-(1-naphthyl)-triphenyl phosphine) nickel match and cocatalyst, methyl aluminoxyane (MAO). Its advantages are simple preparing process, low lost and high catalytic activity.

Description

technical field [0001] The present invention relates to a kind of catalyst system that is used for the polymerization of norbornene and its derivatives, specifically relates to a kind of [2-(2'-substituted-hydroxyphenyl)- 4,5-diphenylimidazole]-(1-naphthyl)-(triphenylphosphine)nickel(II) complex catalyst system. [0002] The present invention also relates to a method for the preparation of the aforementioned catalytic system. [0003] The present invention also relates to the use of the above catalyst system in the polymerization of norbornene and its derivatives. Background technique [0004] Bicyclo[2.2.1]hept-2-ene is commonly known as norbornene. Norbornene and its derivatives can be polymerized in the following three ways: [0005] Polymers with different structures and properties can be obtained by different polymerization methods. The first polymerization method is called ring-opening metathesis polymerization (ROMP), which is the most studied norbornene polymer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/80C08F132/08
Inventor 孙文华杨海健李子龙
Owner INST OF CHEM CHINESE ACAD OF SCI
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