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Preparation method of porous polyquaternary phosphorus ionic liquid

A technology of polyquaternary phosphorus and ionic liquid, applied in the field of material chemistry, can solve problems such as cumbersome methods and inability to realize large-scale production and application

Active Publication Date: 2015-12-09
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(a) M. Armand, F. Endres, D. R. MacFarlane, H. Ohno, B. Scrosati, Nat. Mater. 2009, 8, 621; b) J. H. Cho, J. Lee, Y. Xai, B. Kim, Y. He , M.J.Renn, T.P.Lodge, C.D.Frisbie, Nat.Mater.2008, 7,900; c) F.Liu, L.Wang, Q.Sun, L.Zhu, X.Meng, F.-S.Xiao, J.Am .Chem.Soc.2012,134,16948; d) Y.Xie, Z.Zhang, T.Jiang, J.He, B.Han, T.Wu, K.Ding, Angew.Chem.Int.Ed.2007 , 46,7255.) However, the existing methods for preparing porous polyionic liquids are very cumbersome and cannot be used in large-scale production. The porous polyionic liquid was obtained by melting the hard template and silicon (a) A.Wilke, J.Weber, Macromol. Rapid Commun.2012, 33, 785; b) Q.Li, J.F.Quinn, F.Caruso, Adv.Mater.2005, 17 , 2058; c) Y.J.Wang, A.M.Yu, F.Caruso, Angew.Chem.Int.Ed.2005, 44, 2888; d) J.L.Lutkenhaus, K.McEnnis, P.T.Hammond, Macromolecules 2008, 41, 6047; d) J. . Hiller, J.D. Mendelsohn, M.F. Rubner, Nat. Mater. 2002, 1, 59)

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  • Preparation method of porous polyquaternary phosphorus ionic liquid
  • Preparation method of porous polyquaternary phosphorus ionic liquid
  • Preparation method of porous polyquaternary phosphorus ionic liquid

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preparation example Construction

[0028] The preparation method of the porous polyquaternary phosphine-type ionic liquid includes specific steps: first, the quaternary phosphorus-type ionic liquid as the basic framework material is added to the porogenic solvent, then the polymerization initiator azobisisobutyronitrile is added, and the basic framework material , The mass ratio of the porogenic solvent and the polymerization initiator is 1:2~40:0.003~0.01, then stirred and polymerized at 60°C~240°C for 6~24 hours, and finally recovered the solvent by distillation at 120°C to obtain the porous polyquaternary Phosphorus-type ionic liquid. The prepared porous polyquaternary phosphine ionic liquid has a pore diameter of 0.3-200nm and a specific surface area of ​​370-760m 2 / g between.

[0029] The preparation method of the quaternary phosphorus-type ionic liquid includes: adding vinyl-containing triphenylphosphine and haloalkane to any liquid in toluene, acetone, ethanol or tetrahydrofuran at a molar ratio of 1:1...

Embodiment 1

[0037] Add 100mmol of p-bromostyrene to a tetrahydrofuran solution containing 200mmol of magnesium powder, and stir at room temperature for 3 hours to obtain the Grignard reagent of p-bromostyrene, and then add 50mmol of phenylphosphine dichloride to the above-mentioned in-situ prepared In the Grignard reagent of p-bromostyrene, stir overnight at room temperature. After the reaction was completed, the unreacted Grignard reagent of p-bromostyrene was quenched with saturated ammonium chloride solution, and the obtained product was purified with a silica gel column, and rinsed with an eluent with a volume ratio of petroleum ether and ethyl acetate of 20:1 , to obtain divinyl triphenylphosphine monomer.

[0038] The preparation of vinyltriphenylphosphine and trivinyltriphenylphosphine is carried out according to the above steps respectively, except that 50mmol of phenylphosphine dichloride is replaced by 100mmol of diphenylphosphine chloride or 33mmol of phosphorus trichloride . ...

Embodiment 2

[0040] Add 100mmol of trivinyltriphenylphosphine prepared by the method in Example 1 into 100mL of toluene solution containing 100mmol of p-vinylbenzyl chloride, and reflux at 110°C for 48h, cool to room temperature, and reduce The toluene is evaporated under pressure, and the unreacted reactants of the product obtained are washed away with ether to obtain 4-vinylbenzyl tri-(vinyltriphenyl)phosphorous chloride monomer, whose structure uses figure 1 , figure 2 and image 3 to make sure.

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Abstract

The invention relates to the field of material chemistry and aims to provide a preparation method of a porous polyquaternary phosphorus ionic liquid. The preparation method comprises the following concrete steps: firstly, adding a quaternary phosphorus ionic liquid as a basic framework material into a pore-forming solvent, then, adding azobisisobutyronitrile as a polymerization initiator, and controlling the mass ratio of the basic framework material to the pore-forming solvent to the polymerization initiator at 1:(2-40):(0.003-0.01); then, stirring and polymerizing at the temperature of 60-240 DEG C for 6-24h; and finally, distilling and recovering the solvent at the temperature of 120 DEG C to obtain the porous polyquaternary phosphorus ionic liquid. According to the invention, the porous polyquaternary phosphorus ionic liquid is synthesized through a free radical polymerization one-step method, and no additional monomers are added in the synthesis process, so that the charge density of the porous polyquaternary phosphorus ionic liquid is very high; and different porous polyquaternary phosphorus ionic liquids can be obtained through designing different vinyl functionalized ionic liquid monomers.

Description

technical field [0001] The invention relates to the field of material chemistry, in particular to a method for preparing a porous polyquaternary ionic liquid. Background technique [0002] Compared with porous inorganic materials, porous polymers have advantages in catalysis, adsorption, ion exchange and separation due to their low density, special mechanical properties and high selectivity of monomers that can be adjusted according to requirements. Wide range of applications. (a) N.B.McKeown, P.M.Budd, Chem.Soc.Rev.2006, 35,675; b) P.Kaur, J.T.Hupp, S.T.Nguyen, ACSCatal.2011, 1,819; c) Y.Zhang, S.N.Riduan, Chem.Soc. Rev.2012,41,2083; d) A.Thomas, Angew.Chem.Int.Ed.2010,49,8328; e) Z.Xie, C.Wang, K.E.deKrafft, W.Lin, J.Am.Chem .Soc.2011,133,2056; f) S.-Y.Ding, J.Gao, Q.Wang, Y.Zhang, W.-G.Song, C.-Y.Su, W.Wang, J. Am.Chem.Soc.2011,133,19816; g) P.Zhang, Z.Weng, J.Guo, C.Wang, Chem.Mater.2011, 23, 5243; h) X.Zhu, C.Tian, S.M.Mahurin, S.-H.Chai, C.Wang, S.Brown, G.M.Veith,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F130/02C08J9/28C08L43/02C07F9/54
Inventor 孟祥举孙琦肖丰收
Owner ZHEJIANG UNIV