Catalysis system f nitrogen-phosphinonickel matches and its preparing process and application

A technology of nickel complexes and catalytic systems, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as waste of norbornene resources and achieve raw material Easy to obtain, high catalytic activity, simple to prepare

Inactive Publication Date: 2003-01-15
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
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  • Description
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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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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1.N, the preparation of P ligand: the anhydrous THF solution (10 milliliters (mL)) of (2-methyl)-8-chloroquinoline (1.77 grams (g), 10 millimoles (mmol)) is cooled to -78℃, slowly add PPh dropwise under stirring 2 Li (1.92g, 10mmol) was dissolved in THF (30mL). After dropping, the solution was warmed up to room temperature and reacted for 12 hours. Then heated to 50°C to continue the reaction for 3 hours, the solution was poured into ice water (30mL), extracted with ether (3×30mL), the ether extract was evaporated under reduced pressure to remove about two-thirds of the volume, and the remaining about one-third One of the mother liquors was placed in the refrigerator for 10-16 hours, 2.62g of white crystals were precipitated, the yield: 80%, the melting point was 168°C, the measured values ​​of elemental analysis: C, 80.84; H, 5.58; N, 4.17; C 22 h 18 Theoretical value of NP: C, 80.72; H, 5.54; N, 4.28%; Mass spectrum (EI): m / z 327 (M + , 100%); 1 H NMR (CDCl 3 ): ...

Embodiment 2

[0032] 1. Preparation of the catalyst: at room temperature, NiCl 2 ·6H 2 O (1.18g, 5mmol) was dissolved in 20mL of absolute ethanol, and slowly added dropwise [(2-methyl)-(8-diphenylphosphino)] quinoline (1.64 grams, 5mmol) diethyl ether ( 40mL)-dichloromethane (10mL) solution, during the dropwise addition, light green crystals were precipitated. After the dropwise addition was completed, the reaction was continued for 10 minutes, and then filtered to obtain 1.59 g of light green crystals, with a yield of 70%.

[0033] 2. Norbornene polymerization: vacuumize the dry 250 ml Schlenk bottle with a stirring magnet in turn, and replace it with nitrogen for three times, so that the reaction system is in a nitrogen environment, add 5 μmol [(2-methyl)-( 8-diphenylphosphino)] quinoline nickel(II) chloride, 20 milliliters of toluene, then add 1.00 grams of norbornene (the molar ratio of norbornene monomer to catalyst is 2100), and stir for 5 minutes at 25°C Afterwards, add 3.57 millil...

Embodiment 3

[0035] 1, the preparation of catalyst: preparation method is with embodiment one.

[0036] 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 micromole (μmol) [(2- Methyl)-(8-diphenylphosphino)] quinoline nickel chloride (II), 20 milliliters of toluene, then add 1.00 gram of norbornene (norbornene monomer and catalyst molar ratio is 2100), at 25 After stirring for 5 minutes at ℃, add 5.36 milliliters of procatalyst MAO (MAO / catalyst mol ratio is 1500), react in the time of 25 ℃ after 60 minutes, add 5ml isobutanol to terminate polymerization, add the hydrochloric acid ethanol of 100 milliliters 5‰ again ( volume ratio), stirred at room temperature for 10 hours, then filtered after standing for 2 hours, and the gained polymer was vacuum-dried for 40 hours at 80° C. to obtain 0.4826 grams of polymer, a conversion rate of 48....

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Abstract

A nitrogen-phosphinonickel match catalyst system is composed of the primary catalyst, [(2-methyl)-(8-diphenylphosphino)] nickel quinolinylhalide, and secondary catalyst, methyl aluminoxyane (MAO). Its advantage are low cost, high activity, high output rate of product (norbornaene) (up to 20-100%), and wide range of adjustable molecular weights (1X10 to the power 5-3X10 to the power 6).

Description

technical field [0001] The invention relates to a catalyst system for the polymerization of norbornene and its derivatives, in particular to a nitrogen-phosphine nickel complex catalyst system for the polymerization of norbornene and its derivatives. [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]hex-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 polymerization method. The industrial polynorbornene Norsorex process is...

Claims

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Application Information

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IPC IPC(8): B01J31/16B01J31/24B01J31/28C08F4/70C08G85/00
Inventor 孙文华李子龙杨海健
Owner INST OF CHEM CHINESE ACAD OF SCI
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