Preparation and application of polyamine coordination functional ionic liquid for ATRP reaction
A functional ionic liquid, ionic liquid technology, applied in organic chemistry, bulk chemical production, etc., can solve the problems of difficult separation of catalysts and polymerization products, low ATRP reaction efficiency, low catalyst activity, etc., and achieve easy separation and uniform molecular weight distribution. , the effect of improving the catalytic efficiency
Inactive Publication Date: 2016-11-30
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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Problems solved by technology
The traditional organic ligand has poor compatibility with the ionic liquid solvent system of the reaction, resulting in low catalyst activity, low ATRP reaction efficiency, and difficulty in separating the catalyst from the polymerization product. Therefore, the present invention designs and synthesizes a coordination functional ionic liquid to replace the organic ligand , aiming to solve the shortage of traditional organic ligands in the ATRP reaction of ionic liquid system, the present invention has good application prospects in the field of chemical synthesis in ionic liquids, and meets the development requirements of environmental friendliness
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[0032] 1. Intermediate [R 1 R 3 Synthesis of mim]Cl
[0033] Add 20ml of N-methylimidazole and 40ml of 1,2-dichloroethane into a 100 mL three-necked flask, 2 protection, magnetic stirring in an oil bath at 70°C for 23 h, and then rotary evaporation to remove unreacted 1,2-dichloroethane, followed by extraction of unreacted N-alkylimidazole with ether, this operation was repeated twice, Ether was removed by rotary evaporation again, and finally vacuum-dried for 24h to obtain the intermediate [R 1 R 3 mim]Cl, the yield was 80%.
[0034] [R 1 R 3 mim]Cl is shown by infrared spectrum (FT-IR) figure 1 -a, H NMR spectrum ( 1 HNMR) see figure 2 .
[0035] 2. Polyamine coordination ionic liquid [N 4 Synthesis of MIM]Cl
[0036] Accurately weigh 9g of [R 1 R 3 mim]Cl and 11ml of triethylenetetramine were placed in a 50ml three-necked flask, heated by magnetic force at 70°C for 17h in an oil bath, and then the unreacted organic polyamine was extracted with ethyl acetate. ...
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Belonging to the field of ionic liquid in green chemical industry, the invention specifically relates to synthesis of a polyamine coordination functional ionic liquid for ATRP (atom transfer radical polymerization) reaction. The ionic liquid can coordinate with CuBr to catalyze ATRP reaction in ionic liquid. The steps include: firstly carrying out alkylation reaction on N-alkyl imidazole and 1, 2-dichloroethane to synthesize an intermediate, and then carrying out reaction with aliphatic polyamine to obtain the polyamine coordination functional ionic liquid. The polyamine coordination functional ionic liquid is coordinated with CuBr and then applied to an ionic liquid reaction system to catalyze ATRP reaction, and can achieve good controllability on the ATRP reaction of MMA, and the synthesized polymerization product PMMA has narrow molecular weight distribution (Mw / Mn1.59). The polyamine coordination functional ionic liquid provided by the invention can realize better compatibility of coordination ionic liquid with an ionic liquid solvent system, improves the catalytic activity, enhances the controllability to ATRP reaction, is conducive to separation of the catalyst and the product, and has good application prospects in the field of chemical synthesis in ionic liquid.
Description
technical field [0001] The invention belongs to the field of functional ionic liquids of chemical green reaction systems, and specifically relates to a polyamine coordination functional ionic liquid used for atom transfer radical polymerization (ATRP) reaction and its application. Background technique [0002] ATRP is an active synthesis technology that has developed rapidly in recent years. It uses organic halides as initiators and transition metal complexes as catalysts to catalyze and inhibit the termination reaction using the redox reaction of transition metals. Between active species and dormant species The reversible dynamic equilibrium is established to realize the control of the polymerization reaction process, and various functional polymers with controllable molecular structure and narrow molecular weight distribution can be synthesized. The traditional ATRP reaction is carried out in organic solvents. In recent years, with the increasing requirements for environme...
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IPC IPC(8): C07D233/61C08F120/14C08F4/50
CPCC07D233/61C08F4/50C08F120/14Y02P20/54
Inventor 唐二军薛腾杜煌
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY