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Poly (norbornene-b-polar functionalized norbornene) and preparation method thereof

A technology of norbornene and vinyl norbornene, which is applied in the field of polymer material preparation and can solve the problems of inability to synthesize polynorbornene block copolymers and the like

Active Publication Date: 2022-04-22
NINGBO POLYTECHNIC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the technical problem of not being able to synthesize block copolymers of polynorbornene and polar functionalized polynorbornene in the prior art, the invention provides a poly(norbornene-b-polar functionalized norbornene Bornene) (abbreviated as: P(NB-b-XNB)) and preparation method thereof

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  • Poly (norbornene-b-polar functionalized norbornene) and preparation method thereof
  • Poly (norbornene-b-polar functionalized norbornene) and preparation method thereof
  • Poly (norbornene-b-polar functionalized norbornene) and preparation method thereof

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preparation example Construction

[0033] In a first aspect, the present invention provides a method for preparing poly(norbornene-b-polar functionalized norbornene) (abbreviated as: P(NB-b-XNB)), the method comprising the following steps :

[0034](1) The norbornene solution (solution containing norbornene) is mixed with the ɑ-diimine nickel complex catalyst system to carry out the first polymerization reaction. After a period of polymerization, the norbornene monomer (NB monomer) is completely After the reaction, vinyl norbornene (VNB) is added to carry out the second polymerization reaction to obtain poly(norbornene-b-vinyl norbornene) block copolymer; the present invention adopts α-diimine nickel complex catalyst The system (abbreviated as Ni catalyst) catalyzes the active polymerization of NB and VNB to prepare the block copolymer of NB and VNB, namely poly(norbornene-b-vinylnorbornene), and obtains a gel-free, well-defined The polynorbornene P (NB-b-VNB) that side chain contains vinyl; The poly(norbornen...

Embodiment 1

[0071] At 10°C, add the following formula I to the toluene solution (10 mL) containing NB (0.5 mol / L) in sequence a Shown main catalyst (0.01mmol) and procatalyst sesquiethyl aluminum chloride, the consumption of sesquiethyl aluminum chloride is to make the Al contained in the sesquiethyl aluminum chloride and the Ni contained in the main catalyst The mol ratio is 200, even if the Al / Ni mol ratio is 200, after polymerization reaction 5 hours, sampling is characterized, and finds that NB has completely converted into PNB, and the weight-average molecular weight of PNB (M w ) is 49000g / mol, molecular weight distribution index (M w / M n ) is 1.1. Add 5mmol of VNB to the above polymerization system, after polymerization for 12 hours, add a mass fraction of 5% hydrochloric acid ethanol solution to terminate the reaction, and dry the obtained polymer to constant weight at 40°C to obtain 0.95g block copolymer P( NB-b-VNB), the weight average molecular weight (M of P(NB-b-VNB) w )...

Embodiment 2

[0075] At 20°C, add cocatalyst methylaluminoxane and the following formula I in sequence to a dichloromethane solution (10 mL) containing NB (0.5 mol / L) b For the main catalyst shown (0.015mmol main catalyst), the amount of methylaluminoxane used is such that the molar ratio of Al contained in methylaluminoxane to Ni contained in the main catalyst is 1500, even if the Al / Ni molar ratio is 1500, after polymerization reaction 5 hours, take a sample and carry out characterization, find that NB has completely converted into PNB, the weight-average molecular weight (M of PNB) w ) is 33000g / mol, molecular weight distribution index (M w / M n ) is 1.1. Add VNB 15mmol in above-mentioned polymerization system, after 12 hours of polymerization, add the hydrochloric acid ethanol solution that mass fraction is 5% to stop reaction, the polymer obtained is dried to constant weight at 40 ℃, obtains 1.4g block copolymer P ( NB-b-VNB), the weight average molecular weight (M of P(NB-b-VNB) w...

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Abstract

The invention relates to poly (norbornene-b-polar functionalized norbornene) and a preparation method of the poly (norbornene-b-polar functionalized norbornene). The method comprises the following steps: mixing a norbornene solution with an alpha-diimine nickel complex catalyst system for polymerization, and then adding vinyl norbornene for polymerization to obtain poly (norbornene-b-vinyl norbornene); preparing into a polymer solution, and then adding an initiator and a sulfydryl reagent to carry out sulfydryl-alkene free radical addition reaction to obtain a reaction product solution; and precipitating the reaction product solution in ethanol, and then filtering and drying to obtain the poly (norbornene-b-polar functionalized norbornene). According to the preparation method, a proper alpha-diimine nickel complex catalyst system is adopted for catalyzing living polymerization of norbornene (NB) and vinyl norbornene (VNB) for the first time, P (NB-b-VNB) is obtained, and then the segmented copolymer of norbornene and polar functionalized norbornene is obtained through a click chemical reaction of sulfydryl alkene.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, and in particular relates to a poly(norbornene-b-polar functionalized norbornene) and a preparation method thereof. Background technique [0002] There are three polymerization methods of norbornene, metathesis ring-opening polymerization, addition polymerization and cationic polymerization. Among them, the main chain of polynorbornene (VA-PNB) obtained by addition polymerization is fully saturated, and the structural unit is norbornene with two rings, which has excellent aging resistance, thermal stability and chemical stability. , in addition, the special ring structure endows VA-PNB with high glass transition temperature and excellent transparency, making it widely used in optical materials, film materials, etc. Because the norbornene structural unit is non-polar, its application is limited. The introduction of functional groups on the units of the norbornene structure w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F8/34C08F4/70
CPCC08F293/00C08F8/34C08F4/7006Y02P20/52
Inventor 陈艳君彭振博
Owner NINGBO POLYTECHNIC
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