Functionalized homogeneous particle porous silicon dioxide microspheres and preparation method and application thereof

A technology of porous silica and silica, applied in silica, silica, chemical instruments and methods, etc., can solve the problems of uncontrollable mesopore pore size, too small particle size, uneven particle size of microspheres, etc.

Active Publication Date: 2011-05-25
SUZHOU NANOMICRO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a functionalized uniform particle porous silica microsphere, which solves the problem of uneven particle size or too small particle size or insufficient mesopore diameter of the microsphere obtained by the pr

Method used

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  • Functionalized homogeneous particle porous silicon dioxide microspheres and preparation method and application thereof
  • Functionalized homogeneous particle porous silicon dioxide microspheres and preparation method and application thereof
  • Functionalized homogeneous particle porous silicon dioxide microspheres and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Example 1 Synthesis of homogeneous porous polystyrene / divinylbenzene polymer microspheres

[0063] Take 30 g of styrene, 60 g of divinylbenzene (80%) and 100 g of cyclohexanol into a 2000 mL three-necked round bottom flask, add 1.5 g of azobisisobutyronitrile as an initiator, and mechanically stir to completely dissolve it. Add 800 g of 0.04% sodium octadecyl sulfonate aqueous solution to the above solution, add 25 g of 2.5 μm polystyrene seeds after ultrasonic emulsification, swell at room temperature for 24 hours and then heat to 80°C for reaction. After cooling, the homogeneous porous cross-linked polystyrene microspheres were separated, the particle size was 5 μm, and the coefficient of variation CV=3.5%.

Embodiment 2

[0064] Example 2 Synthesis of homogeneous porous polystyrene / divinylbenzene polymer microspheres

[0065] Take 30 g of styrene, 60 g of divinylbenzene (80%) and 100 g of cyclohexanol into a 2000 mL three-necked round bottom flask, add 1.5 g of azobisisobutyronitrile as an initiator, and mechanically stir to completely dissolve it. Add 800g of 0.04% sodium octadecyl sulfonate aqueous solution to the above solution, add 25g of 5μm polystyrene seeds after ultrasonic emulsification, swell at room temperature for 24 hours and then heat to 80°C for reaction. After cooling, the homogeneous porous cross-linked polystyrene microspheres were separated, the particle size was 10μm, and the coefficient of variation CV=3.5%.

Embodiment 3

[0066] Example 3 Synthesis of homogeneous porous polystyrene / divinylbenzene polymer microspheres

[0067] In a 5 liter reactor, use pre-prepared 60g monodisperse swellable polystyrene particles as seeds, with a particle size of 13.5μm, CV=3.8, and add 1300g of deionized water containing 1g of hydroxypropylcellulose; Stir and heat to 85°C at a speed of rpm.

[0068] After mixing 800g of styrene and 10g of dibenzoyl peroxide, add 1500g of water containing 0.5g of KI, 0.5g of hydroxypropylcellulose and 4.0g of Triton X-405. After mixing, emulsify and increase the rate at 85℃. Add to the aqueous solution, for example, the initial speed is 1ml / min, the final speed is 10ml / min, and the dripping is for a total of 6 hours to carry out the first-stage reaction, and the reaction degree is controlled to be about 80%.

[0069] Add 800g of styrene and 10g of dibenzoyl peroxide into 1500g of water containing 0.5g of hydroxypropylcellulose and 4.0g of TritonX-405, mix and emulsify, adjust the temp...

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Abstract

The invention discloses functionalized homogeneous particle porous silicon dioxide microspheres and a preparation method and application thereof. The preparation method comprises the following steps of: (1) pre-preparing homogeneous particle porous polymer microspheres with determined components, particle diameters and apertures, and performing surface functionalized treatment on the porous polymer microspheres to obtain the functionalized homogeneous particle porous polymer microspheres; (2) dispersing the functionalized porous polymer microspheres in aqueous solution and adding silicon dioxide precursor to prepare silicon dioxide/polymer intermediate composite microspheres; (3) heating the silicon dioxide/polymer intermediate composite microspheres to remove the polymer to obtain the homogeneous particle porous silicon dioxide microspheres; and (4) performing surface modification on the homogeneous particle porous silicon dioxide microspheres by using a chemical reagent to form a functionalized group, wherein the particle diameter of the functionalized homogeneous particle porous silicon dioxide microspheres is within the range of between 1.7 and 100 microns; and the mesoporous aperture of the functionalized homogeneous particle porous silicon dioxide microspheres is within the range of between 20 and 1,000 angstroms. The functionalized homogeneous particle porous silicon dioxide microspheres can be used as chromatographic filler for efficiently analyzing and separating organic molecules and biological molecules.

Description

Technical field [0001] The invention belongs to the field of column packing preparation technology and its application in liquid chromatography technology, and specifically relates to a preparation method and application of micron-level functional homogeneous porous silica microspheres. Background technique [0002] Micron-sized porous silica microspheres have a wide range of applications in many fields such as analysis, catalysis and separation. Due to its high mechanical strength, heat resistance, and solvent resistance, it is often used as a support framework for catalytic conversion, enzyme immobilization and liquid chromatography. With the development of high performance liquid chromatography technology, the particle size and pore structure of porous silica microspheres need to be precisely controlled, and the particle size needs to be controlled between 3 and 10 microns, and the pore surface needs to have a certain Hydrophobicity. In terms of chromatographic performance, ...

Claims

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Application Information

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IPC IPC(8): C01B33/12B01J20/10B01J20/30B01D15/08
Inventor 江必旺吴俊成陈荣姬
Owner SUZHOU NANOMICRO TECH CO LTD
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