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Preparation method of porous polyquaternary phosphorus ionic liquid

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

Active Publication Date: 2013-12-11
ZHEJIANG UNIV
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  • 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, such as post-grafting ionic liquids on the original porous polymers, and nano Silicon spheres are used as hard templates and porous polyionic liquids are obtained by melting silicon ( a) A. Wilke, J. Weber, Macromol. Rapid Commun. 2012, 33, 785; b) Q. Li, J. F. Quinn, F. Caruso, 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)

Method used

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  • Preparation method of porous polyquaternary phosphorus ionic liquid
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[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 Porous polyquaternary 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 to 10 and stirred ...

Embodiment 1

[0037] Add 100 mmol of p-bromostyrene to a tetrahydrofuran solution containing 200 mmol of magnesium powder, and stir at room temperature for 3 hours to obtain the Grignard reagent of p-bromostyrene, and then add 50 mmol of phenylphosphine dichloride to the above in situ The prepared p-bromostyrene Grignard reagent was stirred 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] The 100 mmol trivinyltriphenylphosphine prepared by the method in Example 1 was added to 100 mL of toluene solution containing 100 mmol p-vinylbenzyl chloride, and refluxed at 110 ° C for 48 h, cooled to room temperature, and Evaporate the toluene under reduced pressure with the evaporator, and wash the unreacted reactant with diethyl ether to obtain 4-vinylbenzyl tri-(vinyltriphenyl) phosphorus chloride monomer, whose structure is 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, ACS Catal. 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 ...

Claims

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Application Information

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