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Porous silica gel used as liquid chromatography stationary phase material and preparation method thereof

A technology of porous silica gel and liquid chromatography, used in chemical instruments and methods, other chemical processes, etc., can solve the problems of backward preparation methods and poor packing performance.

Inactive Publication Date: 2014-04-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is still a large gap between domestic fillers and foreign developed countries in terms of performance and variety, mainly reflected in two aspects: backward preparation methods and poor filler performance.

Method used

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  • Porous silica gel used as liquid chromatography stationary phase material and preparation method thereof
  • Porous silica gel used as liquid chromatography stationary phase material and preparation method thereof
  • Porous silica gel used as liquid chromatography stationary phase material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Dissolve 2g of PVP in a mixed solvent consisting of ethanol (60g) and water (8g), put it into a 250ml four-necked flask equipped with a thermometer, agitator and condenser, pass nitrogen protection, and pre-disperse at 70℃ for 30min , Then add monomer St (30g) and initiator AIBN (0.3g), react at 70℃ for 12h. Centrifuge the resulting product in a 10000r / s ultracentrifuge for 10 minutes. Wash the precipitate with 95% ethanol, then settle again to remove the supernatant. The above operations are repeated twice and then dried at room temperature to a milky white polystyrene powder Store at low temperature.

[0028] After dissolving 2g of PEI in water to make a 2% aqueous solution, add 1g of PS sample and magnetically stir for 6 hours.

[0029] Add 20g of ethyl silicate, 6g of nitric acid, and 14g of distilled water into a 250ml beaker, and stir evenly until no layering occurs. Add 18.8g VTMS, continue to stir, when it becomes a sol, add 0.4g of PSPEI (ie polystyrene wrapped wi...

Embodiment 2

[0032] The preparation steps of the polystyrene microspheres and the encapsulated PEI in this embodiment are the same as those in the first embodiment. The difference is: add 10g of ethyl silicate, 3g of nitric acid, and 7g of distilled water into a 250ml beaker, and stir evenly until no layering occurs. Add 9.4g VTMS, continue stirring, when it becomes a sol, add 0.4g PS-PEI, continue stirring until it becomes a gel, stop stirring, and obtain a sandy polystyrene / polysiloxane gel composite.

[0033] Soak the polystyrene / polysiloxane gel composite obtained in the previous step with dimethylformamide for 10 minutes, put it in the reaction kettle and put it in the oven, set the temperature to 120℃, and the time to 4 hour. After the sample was taken out, it was put into a beaker, dissolved in DMF and continuously stirred, and repeatedly filtered with a water pump to finally obtain a white porous polysiloxane.

Embodiment 3

[0035] The preparation steps of the polystyrene microspheres and the encapsulated PEI in this embodiment are the same as those in the first embodiment. The difference is: add 5g ethyl silicate, 1.5g nitric acid, and 3.5g distilled water into a 250ml beaker, and stir evenly until no layering occurs. Add 4.7g VTMS, continue stirring, add 0.4g PS-PEI when it becomes a sol, continue stirring until it becomes a gel, stop stirring, and obtain a sandy polystyrene / polysiloxane gel composite.

[0036] Soak the polystyrene / polysiloxane gel composite obtained in the previous step with dimethylformamide for 15 minutes, put it in the reaction kettle and put it in the oven, set the temperature to 150°C, and the time to 4 hour. After the sample was taken out, it was put into a beaker, dissolved in DMF and continuously stirred, and repeatedly filtered with a water pump to finally obtain a white porous polysiloxane.

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Abstract

The invention discloses porous silica gel used as a liquid chromatography stationary phase material and a preparation method thereof. The method comprises the following steps: firstly preparing a polystyrene microsphere template by dispersion polymerization, then coating polyethylene imine on the polystyrene surface to let the polystyrene microsphere surface have positive charges, preparing polystyrene coating polyethylene imine / polysiloxane gel by sol-gel process, and finally removing the polystyrene template in the complex by using solvent thermal treatment. The preparation method disclosed in the invention is an innovation based on the existing preparation method, has simple operation and easiness in control, the specific surface area of the porous silica gel matrix is large, thus mass transfer is benefited, the operation pressure can be reduced, the particle size is 2-3 mum, the synthetic process is simple, and the advantages of existing porous silica gel are kept in the respect of packing performance and are greatly improved in the respects of specific surface area and low pressure operation.

Description

Technical field [0001] The invention belongs to a liquid chromatography stationary phase synthesis technology, and more specifically, relates to a porous silica gel microsphere and a preparation method thereof. Background technique [0002] Chromatography is an important method for the analysis of biological substances. With the continuous increase of analysis objects and the increasing complexity of samples, the requirements for chromatographic technology are also increasing. Among them, the packing of the chromatographic column is very important to the chromatographic separation and is the key to effective separation. The ideal column packing should have a narrow particle size distribution, a higher specific surface area and a suitable pore structure, as well as stable chemical properties and mechanical strength. The pore size is the key factor that affects the separation effect of the chromatographic packing. The pore size determines the specific surface area of ​​the chromat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/283B01J20/30
Inventor 龚彩荣邵莹李雪云敖敏范国樑
Owner TIANJIN UNIV
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