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Norbornene polymerization catalyst system and its preparing process

A technology for 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, and the field of two-nickel complex catalytic systems, which can solve the waste of norbornene resources and other problems, to achieve the effects of good stability, simple preparation and easy availability of raw materials

Inactive Publication Date: 2003-01-01
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

[0032] 1.O, N, the preparation of O tridentate salicylaldehyde-o-methoxyaniline Schiff base ligand: 3 millimoles (mmol) of salicylaldehyde and 3 millimoles (mmol) of o-aminophenyl formazan Base ether (o-aminoanisole) was placed in a 25 milliliter (mL) Erlenmeyer flask, placed in a microwave oven, and reacted for 30 seconds at a power of 616W, then left to stand, and after the reaction system was solidified into a solid, use ethanol After recrystallization, a yellow Schiff's base product was obtained with a yield of 98%. Elemental analysis measured values: C, 83.57; H, 5.98; N, 4.88; O, 5.57%; C 14 h 13 NO 2 Theoretical value of: C, 83.59; H, 5.96; N, 4.87; O, 5.57%; 1 HNMR (CDCl 3 ): 3.89(s, 1H), 6.92-7.41(m, 8H), 8.71(s, 1H), 13.89(s, 1H); 13 CNMR (CDCl 3 ): 56.1(1C), 115.5(1C), 115.9(1C), 118.5(1C), 121.3(1C), 122.2(1C), 128.4(1C), 128.5(1C), 130.6(1C), 133.2(1C ), 139.9(1C), 155.6(1C), 158.1(1C), 165.7(1C).

[0033] 2. Preparation of catalyst:

[0034] Dissolve 2 m...

Embodiment 2

[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, add 5 μmol of the catalyst prepared in step 1, 20 ml Toluene, then add 4.708 gram of norbornene (norbornene monomer and catalyst molar ratio is 10000), after stirring for 5 minutes at 25 ℃, add 5.3 milliliters of procatalyst MAO (MAO / catalyst molar ratio is 1500), at 25 After reacting for 30 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 1.0833 grams of polymer, a conversion rate of 23.01%, and a catalyst activity of 4.3×10 5 gPNB / (molNi h atm). Polymer weight ...

Embodiment 3

[0040] 1, the preparation of catalyst: preparation method is with embodiment one.

[0041] 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 4.708 grams of norbornene (norbornene monomer and catalyst molar ratio is 10000), after stirring for 5 minutes at 25 ℃, add 1.8 milliliters of procatalyst MAO (MAO / catalyst molar ratio is 500), after reacting for 30 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 for 40 hours at 80° C. to obtain 0.0711 grams of polymer, the conversion rate was 1.51%, and the catalyst activity was 2.84×10 4 gPNB / (mol...

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Abstract

The oxygen-nitrogen-oxygen nickel compound catalyst system for polymerization of norbornene consists of di(substituted salicylal-substituted o-alkoxy anilino schiff base) nickel (II) compound as main catalyst component and methyl aluminoxane as cocatalyst. It has simple preparation process, low cost, high catalytic activity up to 6.8x10E8 g PNB / mol Ni.hr, and the product polynorbornene has molecular weight adjustable in wide range of 10E5 to 3.4x10E6 and molecular weight distribution adjustable in wide range of 1.1-20 through altering the activity of catalyst and other reaction conditions. The yield of polynorbornene in 20-100%.

Description

technical field [0001] The invention relates to a catalytic system for the polymerization of norbornene and its derivatives, in particular to a bis(substituted salicylaldehyde-substituted o-alkoxyaniline) used for the polymerization of norbornene and its derivatives Buddha alkali) nickel (II) complex catalytic 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 p...

Claims

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Application Information

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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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