Preparation method of grafted quaternary phosphonate ionic liquid

An ionic liquid and quaternary phosphine technology, which is applied in the field of preparation of grafted quaternary phosphine type ionic liquids, can solve the problems of weak physical force and loss of ionic liquid, and achieves good adsorption performance, good CO2 adsorption performance, and large cumulative specific surface area. Effect

Inactive Publication Date: 2012-07-18
CHINA UNIV OF MINING & TECH
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Problems solved by technology

At present, the physical impregnation method is commonly used to prepare immobilized ionic liquids, which cannot overcome the gaps filled by ionic liquids into the carrier, resulting in blocked pores, hindering the transfer of CO 2 in the pores and affecting CO 2 adsorption efficiency, and the simple physical force between the ionic liqu...

Method used

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  • Preparation method of grafted quaternary phosphonate ionic liquid
  • Preparation method of grafted quaternary phosphonate ionic liquid
  • Preparation method of grafted quaternary phosphonate ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0018] The synthesis of embodiment 1 chloride quaternary phosphine ionic liquid intermediate (II)

[0019] Add 20ml of anhydrous toluene into the three-necked flask, N 2 Protection; add 3.0g 3-chloropropyltriethoxysilane (I) into toluene with a syringe, then add 6.0g trioctylphosphine in the same way; heat and reflux in an oil bath at 120°C for 24h; react The product was allowed to stand, and the layers were separated. The ionic liquid phase was taken and washed three times with ether to remove toluene and unreacted substances; vacuum-dried at 80°C for 24 hours to obtain the brown-yellow quaternary phosphine chloride ionic liquid intermediate (Ⅱ).

Embodiment 2 4

[0020] Example 2 Synthesis of Tetrafluoroboric Acid Ionic Liquid Intermediate (Ⅲ)

[0021] Put 1.9 g of the quaternary phosphine chloride ionic liquid intermediate (II) obtained in the previous step into a three-necked flask, then add 0.6 g (excess) sodium tetrafluoroborate into the flask under constant stirring, and then add 150 mL acetonitrile, stirred and reacted for 35 h; the two salts gradually dissolved and a new white precipitate was formed. Since the precipitates before and after the reaction were all white, the reaction process was not obvious; the precipitate was removed by filtration, and about 750 mL of ether was added to the filtrate. White crystals were formed; the white precipitate was obtained by filtration, and vacuum-dried at room temperature for 10 h to obtain tetrafluoroborate ionic liquid intermediate (Ⅲ).

Embodiment 3

[0022] Example 3 Synthesis of grafted quaternary phosphine-type ionic liquid (IV)

[0023] Calcinate the silica carrier at 550°C for 6 hours, add 150ml of toluene to the flask, add 1.6 g of tetrafluoroborate ionic liquid (Ⅲ) into the toluene, and use N 2 Exhaust the air; add 2.0 g carrier, and stir the reaction mixture at 90°C for 3h; vacuum dry at 110°C for 2h to obtain the final product grafted quaternary phosphine-type ionic liquid (Ⅳ) particles.

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Abstract

The invention relates to a preparation method of a grafted quaternary phosphonate ionic liquid. The preparation method comprises the following steps of: using 3-(chloropropyl)triethoxysilane and trioctylphosphine to react and generate a chlorinated quaternary phosphonate ionic liquid intermediate, then using the chlorinated ionic liquid intermediate and sodium fluoroborate to synthesize a tetrafluoroborate quaternary phosphonate ionic liquid intermediate, and finally using the tetrafluoroborate ionic liquid intermediate and silica to react and generate the grafted quaternary phosphonate ionic liquid. The grafted quaternary phosphonate ionic liquid provided by the preparation method of the grafted quaternary phosphonate ionic liquid can be used as the CO2 adsorbent alone and can also be used along with other adsorption materials; and compared with the silica gel supported 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid which is synthesized by the traditional immersion method and the silica gel supported 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid which is synthesized by the sol-gel method, the grafted quaternary phosphonate ionic liquid has larger cumulative specific surface area and better CO2 adsorption property.

Description

technical field [0001] The invention relates to a preparation method of an ionic liquid in the fields of organic chemistry and chemical engineering, in particular to a preparation method of a grafted quaternary phosphine-type ionic liquid. Background technique [0002] With the development of industry, the CO emitted into the atmosphere after humans use fossil fuels 2 With each passing day, global environmental problems are becoming more and more serious. Countries are working to control and reduce CO 2 emissions, the development of adsorptive separation of CO 2 Technology is a hot spot of common concern around the world. Currently CO 2 The capture methods mainly include solvent absorption, pressure swing adsorption and membrane separation, etc. Among them, the organic amine aqueous solution absorption method is the most common, but because the organic amine aqueous solution is volatile, it is easy to produce secondary pollution of VOCs. The adsorption metho...

Claims

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Application Information

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IPC IPC(8): B01D53/14
CPCY02A50/20
Inventor 朱佳媚张虎何凯歌辛丰孙雅钗
Owner CHINA UNIV OF MINING & TECH
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