Nickel compound catalyst system for polymerization of norbornene and its prepn

A technology of norbornene and nickel complexes, applied in the catalytic system of []nickel complexes, the application of the above-mentioned catalytic system in the polymerization of norbornene and its derivatives, the preparation field of the above-mentioned catalytic system, can solve the problem of norbornene Waste of resources and other issues, to achieve the effect of good stability, high catalytic activity, and easy access to 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 i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Preparation of N, O bidentate salicylaldimine ligand: In a 250 milliliter (mL) round bottom flask, mix 3 millimoles (mmol) of 2-hydroxyl-3,5-diiodobenzaldehyde with 3 millimoles (mmol) of 2,6-diisopropylaniline was dissolved in 50 milliliters of absolute ethanol, stirred and refluxed for 4.5 hours, and left to cool to room temperature to obtain a yellow Schiff base product, which was separated by silica gel column chromatography with a yield of 87 %. Elemental analysis measured values: C, 42.81; H, 3.95; I, 47.61; N, 2.62; O, 3.01%; 19 h 21 I 2 Theoretical value of NO: C, 42.80; H, 3.97; I, 47.60; N, 2.63; O, 3.00%; 1 H NMR (CDCl 3 ): 1.16-1.19(d, 12H), 2.95-3.02(m, 2H), 6.92-7.88(m, 5H), 8.51(s, 1H), 13.56(s, 1H); 13 CNMR (CDCl 3 ): 23.6(2C), 24.8(4C), 86.5(1C), 92.0(1C), 121.3(1C), 124.2(2C), 126.3(1C), 138.5(1C), 141.8(2C), 148.5(1C ), 150.2(1C), 163.5(1C), 165.6(1C).

[0032] 2. Preparation of catalyst:

[0033] Dissolve 2 mmoles of the yellow Schiffer b...

Embodiment 2

[0036] 1, the preparation of catalyst: preparation method is with embodiment one.

[0037] 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, 30 ml Toluene, then add 4.708 gram of norbornene (norbornene monomer and catalyst mol ratio is 10000), after stirring for 5 minutes at 25 ℃, add 4.3 milliliters of procatalyst MAO (MAO / catalyst mol ratio is 1200), 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 yielded 3.0150 grams of polymer, a conversion rate of 64.04%, and a catalyst activity of 1.3×10 6 gPNB / (molNi h atm). Polymer weight a...

Embodiment 3

[0039] 1, the preparation of catalyst: preparation method is with embodiment one.

[0040] 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 3.6 milliliters of procatalyst MAO (MAO / catalyst molar ratio is 1000), after reacting for 30 minutes at 25°C, 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 to obtain The polymer was vacuum-dried at 80°C for 40 hours to obtain 3.6753 grams of polymer, the conversion rate was 78.06%, and the catalyst activity was 1.47×10 6 gPNB / (...

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Abstract

The nitrogen-oxygen nickel compound catalyst system for polymerization of norbornene consists of di(substituted salicylal-substituted anilino schiff base) (1-naphthyl)(triphenyl phosphine) nickel (II) compound as main catalyst component and methyl aluminoxane as cocatalyst. It has simple preparation process, low cost, high catalytic activity up to 1.03x10E9 g PNB/ mol Ni.hr.atm, and the product polynorbornene has molecular weight adjustable in wide range of 10E5 to 3.7x10E6 and molecular weight distribution adjustable in wide range of 1.3-23 through altering the activity of catalyst and other reaction conditions. The yield of polynorbornene is 20-100%.

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 [(substituted salicylaldehyde-substituted aniline Schiff base) ( 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 application 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 norb...

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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