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Catalysis system of nitrogen-accessory ingredient of oxygen and nickel in use for polymerizaton of norborene and ramification, preparation method and application

A norbornene and catalytic system technology, applied in the field of nitrogen-oxygen nickel complex catalytic system and preparation thereof, can solve problems such as waste of norbornene resources, and achieve the effects of easy availability of raw materials, simple preparation and high catalytic activity

Inactive Publication Date: 2005-01-12
YINGKOU XIANGYANG CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 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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  • Catalysis system of nitrogen-accessory ingredient of oxygen and nickel in use for polymerizaton of norborene and ramification, preparation method and application
  • Catalysis system of nitrogen-accessory ingredient of oxygen and nickel in use for polymerizaton of norborene and ramification, preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1.N, the preparation of O ligand: 3 millimoles (mmol) 4,5-diazafluoren-9-ketones are dissolved in 30 milliliters (ml) absolute ethanol, and add the p-toluene of catalytic amount Sulfonic acid, reflux and stir for 10 minutes; add 3 mmoles of benzoylhydrazide to the absolute ethanol solution of 4,5-diazafluoren-9-one; reflux and stir for 5 hours, concentrate the solution to the original 1 / 3. Filter to obtain a yellow-white precipitate. The yellow-white precipitate was recrystallized in absolute ethanol to obtain yellow-white crystals. Yield: 90%, product confirmation: EI-MS (m / z): 30O (M + , 61.0%), 197 (15.7%), 181 (16.9%), 169 (13.7%), 154 (7.9%), 139 (3.6%), 122 (10.1%), 105 (100%), 94 (5.6 %), 77 (33.7%).

[0028] 2. Preparation of catalyst: under reflux, dissolve 1 mmol of the above-mentioned yellow Schiff base in 15 milliliters of absolute ethanol, then add dropwise 10 milliliters of absolute ethanol solution with 0.5 mmol of nickel acetate tetrahydrate, and rea...

Embodiment 2-7

[0031] Embodiment 2-embodiment 7 N, the preparation of O ligand and catalyst are identical with embodiment 1, and the conditions and the result of norbornene polymerization are shown in Table 1:

[0032] Reality

Embodiment 8

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

[0035] 2. Norbornene polymerization: Vacuumize the dry 100 ml Schlenk bottle with a stirring magnet, and replace it with nitrogen three times, so that the reaction system is in a nitrogen environment, add 5 μmol of the catalyst described in step 2, and 19.32 ml of toluene , then add 3.89 milliliters of toluene solution containing 2.3538 grams of norbornene (norbornene monomer and catalyst molar ratio is 5000), after stirring for 5 minutes at 25 ℃, add 1.79 milliliters of procatalyst MAO (MAO / catalyst molar ratio is 500), after reacting for 240 minutes at 25°C, add 15 milliliters of isobutanol to terminate the polymerization, then add 80 milliliters of 5‰ hydrochloric acid ethanol (volume ratio), stir at room temperature for 10 hours, then filter after standing for 2 hours, Gained polymer was vacuum-dried at 80° C. for 48 hours to obtain 1.54 grams of polymer, with a conversion rate of 65.6%, an...

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Abstract

The invention provides a nitrogen-oxynickel complex catalytic system for polymerization of norbornene and its derivative, its preparation method and application. Said catalytic system for polymerization is formed from main catalyst nitrogen-oxynickel complex-bis (4,5-diazafluorene-9-ketone substituted benzoyl hydrazone) II nickel dihydrate (A) or brominated bis (2-pyridylaldehyde substituted benzoyl hydrazone) II nidal (B) and auxiliary catalyst methylaluminoxane. The preparation method of main catalyst nitrogen-oxynickel complex includes the following steps: firstly, using substituted benzoyl hydrazine and 4,5-diazafluorene-9-ketone or 2-pyridylaldehyde to prepare N,O bidenate, then making the the ligand and tetrahydrate nickel acetate or 1,2-dimethoxyethane nickel bromide product reaction so as to respectively obtain the main catalyst (A) or (B). Said invention process is simple, its raw materials are easily available, the use level, methylaluminoxane is low, and the yield rate of polynorbornene and its derative can be up to 20-100%.

Description

technical field [0001] The invention relates to a nitrogen-oxygen nickel complex catalyst system used in the polymerization of norbornene and its derivatives in high molecular polymers, as well as its preparation method and application. Background technique [0002] Bicyclo[2,2,1]hept-2-ene is commonly known as norbornene. Norbornene and its derivatives can be polymerized in three ways as shown in the figure below [0003] [0004] Polymers with different structures and properties can be obtained by different polymerization methods. The first polymerization method is called ring-opening metathesis polymerization (ROMP). The resulting polymer chain still contains double bonds, so it can be processed into materials suitable for different purposes by hydrogenation or cross-linking. It is the most studied type of norbornene The industrial polynorbornene Norsorex process is the application of ROMP in actual production. Little is known about the second polymerization method ...

Claims

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Application Information

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IPC IPC(8): C08F4/602C08F32/08
Inventor 孙文华赵东风侯俊先李伟张东恒
Owner YINGKOU XIANGYANG CATALYST
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