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Preparation method of superhigh-specific-area monodisperse polymer microspheres

An ultra-high specific surface area, monodisperse technology, which is applied in the field of preparation of monodisperse polymer microspheres, can solve the problems that the specific surface area of ​​the product is not given, and there is little attention to the preparation of ultra-high specific surface area microspheres.

Active Publication Date: 2013-06-19
嘉善县国创新能源研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent CN101864020 discloses a method for preparing highly cross-linked polystyrene microspheres by dispersion polymerization. This patent uses styrene and divinylbenzene as monomers, and adds polymerizable ionic monomers as stabilizers. Monodisperse highly cross-linked polystyrene microspheres were prepared by one-pot method, but the specific surface area of ​​the product was not given in the patent
[0007] However, the ultra-high specific surface area microspheres prepared in the current published literature and patents all have different degrees of agglomeration, and little attention has been paid to the preparation of submicron ultra-high specific surface area microspheres

Method used

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  • Preparation method of superhigh-specific-area monodisperse polymer microspheres
  • Preparation method of superhigh-specific-area monodisperse polymer microspheres
  • Preparation method of superhigh-specific-area monodisperse polymer microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a 250mL three-neck flask equipped with an argon gas line, mechanical stirring and condenser, add 9.5mL vinylbenzyl chloride (VBC), 0.5mL divinylbenzene (DVB), 0.1g cetyl alcohol (CA) , 100mL of deionized water and 0.132g of azobisisobutylamidine hydrochloride (AIBA), cooled in an ice bath, ultrasonically dispersed for 150s with a JY92 cell pulverizer, and the output power was 40%, and then quickly transferred to a heating oil bath, Heating to 70°C for 12 hours, the product was centrifuged and washed, then dried in a vacuum oven for 24 hours.

[0022] In a 250 mL three-neck flask equipped with an argon gas line, mechanical stirring and condenser, add 1.5 g of prepolymer microspheres, 120 mL of dichloromethane and 0.6 g of FeCl 3 , swelled and stirred at room temperature for 24 hours, then rapidly heated to 80 ° C for 8 hours, and after centrifugation, the product was washed with methanol, dilute nitric acid solution and deionized water, and dried in vacuum. The speci...

Embodiment 2

[0024] In a 250mL three-neck flask equipped with an argon gas line, mechanical stirring and condenser, add 9.0mL vinylbenzyl chloride (VBC), 0.5mL divinylbenzene (DVB), 0.5mL hydroxyethyl acrylate, 0.1g Cetyl alcohol (CA), 100mL deionized water and 0.132g azobisisobutylamidine hydrochloride (AIBA), cooled in an ice bath, ultrasonically dispersed for 150s with a JY92 cell pulverizer, output power 40%, and then quickly Transfer to a heating oil bath, heat to 70°C and react for 12 hours. After the product is centrifuged and washed, it is dried in a vacuum oven for 24 hours.

[0025] In a 250 mL three-neck flask equipped with an argon gas line, mechanical stirring and condenser, add 1.8 g of prepolymer microspheres, 120 mL of dichloromethane and 0.5 g of AlCl 3 , swelled and stirred at room temperature for 24 hours, then rapidly heated to 80 ° C for 8 hours, and after centrifugation, the product was washed with methanol, dilute nitric acid solution and deionized water, and dried i...

Embodiment 3

[0027] In a 250mL three-neck flask equipped with an argon gas line, mechanical stirring and condenser, add 8.0mL vinylbenzyl chloride (VBC), 0.5mL divinylbenzene (DVB), 1.5mL styrene, 0.1g hexadecane Alkanol (CA), 100mL deionized water and 0.132g azobisisobutylamidine hydrochloride (AIBA), cooled in an ice bath, ultrasonically dispersed for 150s with a JY92 cell pulverizer, output power 40%, and then quickly transferred to In a heating oil bath, heat to 70°C to react for 12 hours. After the product is centrifuged and washed, it is dried in a vacuum oven for 24 hours.

[0028] In a 250 mL three-neck flask equipped with an argon gas line, mechanical stirring and condenser, add 2.1 g of prepolymer microspheres, 120 mL of dichloromethane and 0.9 g of SnCl 4 , swelled and stirred at room temperature for 24 hours, then rapidly heated to 80 ° C for 8 hours, and after centrifugation, the product was washed with methanol, dilute nitric acid solution and deionized water, and dried in va...

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Abstract

The invention provides a method for preparing superhigh-specific-area monodisperse polymer microspheres, which comprises the following steps: adding monomer, divinylbenzene, vinyl benzyl chloride, deionized water, initiator azodiisobutylamidine hydrochloride and co-stabilizer cetyl alcohol into a reaction vessel, carrying out ultrasonic dispersion in a cell crusher for 3 minutes, heating to 70 DEG C, reacting for 12 hours, centrifuging, washing and drying to obtain lightly-crosslinked monodisperse prepolymer microspheres; and swelling the monodisperse prepolymer microspheres, dispersion medium and Lewis acid catalyst at room temperature for 24 hours, heating to 80 DEG C, reacting for 8 hours, centrifuging, washing and drying to obtain the superhigh-specific-area monodisperse polystyrene microspheres. The particle size of the polystyrene microspheres is 600-750 nm, and the particle size distribution coefficient is less than 8.5; the maximum specific area can reach 1255 m<2> / g, and the maximum pore volume can reach 0.78 cm<3> / g; the average pore size is 2.3-2.7 nm, and the pore size distribution is narrow; and the maximum adsorption capacity for hydrogen can reach 2.15 wt%.

Description

technical field [0001] The invention belongs to the field of polymer material preparation, and in particular relates to a method for preparing monodisperse polymer microspheres with an ultrahigh specific surface area. Background technique [0002] Monodisperse polymer microspheres with ultra-high specific surface area have good swelling ability in both good thermodynamic solvents and poor solvents. Therefore, such materials are widely used in the fields of hydrogen storage, high performance liquid chromatography, special adsorption and nanomaterial growth templates. There are potential application prospects. [0003] Through the two-step method of prepolymer preparation and post-crosslinking or obtaining polymer materials with ultra-high specific surface area, Davankov et al. have done a lot of pioneering work in this field (J. Chromatogr. A 2002, 965, 65), Sherrington et al. have also done fruitful work in this field, using precipitation polymerization and emulsion polymer...

Claims

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Application Information

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IPC IPC(8): C08F212/14C08F212/36C08F212/08C08F220/06C08F220/28C08F220/56C08F220/34C08F2/22C08J3/24
Inventor 刘清泉唐哲廖博
Owner 嘉善县国创新能源研究院
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