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Preparation method of functional inorganic silicon-based chiral microsphere fixed-phase material based on amylose derivatives

An amylose and functionalization technology, applied in the field of preparation of chiral microsphere stationary phase materials, can solve the problems of reduced separation efficiency, tailing, low yield, etc. Effect

Inactive Publication Date: 2017-01-04
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction process of this material is not easy to control, resulting in low yield and poor repeatability
In addition, since the hybrid microspheres were not processed accordingly, there were a large number of silanol groups on the surface of the material, which made the material appear more obvious tailing phenomenon when it was used for chromatographic separation, greatly reducing its separation efficiency
Up to now, there has been no research on the new preparation method of this kind of organic-inorganic hybrid material and its tailing problem, as well as the research on the preparation of this type of organic-inorganic hybrid material based on other types of polymers (such as amylose derivatives). See the report

Method used

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  • Preparation method of functional inorganic silicon-based chiral microsphere fixed-phase material based on amylose derivatives
  • Preparation method of functional inorganic silicon-based chiral microsphere fixed-phase material based on amylose derivatives
  • Preparation method of functional inorganic silicon-based chiral microsphere fixed-phase material based on amylose derivatives

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Experimental program
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Effect test

specific Embodiment approach 1

[0017] 1. Take 0.2g of microcrystalline amylose and vacuum-dry at high temperature for 4h, then stir and reflux in anhydrous N,N-dimethylacetamide for 12h; add lithium chloride after cooling to room temperature (the mass is the mass of amylose After stirring for 3 hours, heat up again, add anhydrous pyridine, add an appropriate amount of 3,5-dimethylphenyl isocyanate (77mol% of the amylose hydroxyl group) after 2 hours of reflux, continue stirring and reflux for 8 hours, and then add a small amount of 3-(trimethoxysilyl) propyl isocyanate (3.1mol% of amylose hydroxyl group), continued to stir and reflux for 12h and then treated with excess 3,5-dimethylphenylisocyanate (90mol% of amylose hydroxyl group ), continue to stir and reflux for 8 hours, then stop the reaction; cool to room temperature, add methanol to settle, filter and wash, and vacuum-dry at 60°C to constant weight, with a yield of 87%. The introduction ratio of 3,5-dimethylphenyl carbamate to 3-(trimethoxysilyl)prop...

specific Embodiment approach 2

[0022] 1. Take 0.2g of microcrystalline amylose and vacuum-dry at high temperature for 4h, then stir and reflux in anhydrous N,N-dimethylacetamide for 12h; add lithium chloride after cooling to room temperature (the mass is the mass of amylose After stirring for 3 hours, heat up again, add anhydrous pyridine, add an appropriate amount of 3,5-dimethylphenyl isocyanate (77mol% of the amylose hydroxyl group) after 2 hours of reflux, continue stirring and reflux for 8 hours, and then add a small amount of 3-(trimethoxysilyl)propyl isocyanate (6.9mol% of amylose hydroxyl group) was treated with excess 3,5-dimethylphenylisocyanate (90mol% of amylose hydroxyl group) after continuous stirring and reflux for 12h , continue to stir and reflux for 8h to stop the reaction; cool to room temperature, add methanol to settle, filter and wash, vacuum dry at 60°C to constant weight, and the yield is 85%. The introduction ratio of 3,5-dimethylphenyl carbamate to 3-(trimethoxysilyl)propyl carbama...

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Abstract

The invention provides a preparation method of a functional inorganic silicon-based chiral microsphere fixed-phase material based on amylose derivatives. The preparation method comprises the following steps: taking amylose as an initial raw material; simultaneously introducing 3,5-dimethylphenylcarbamate and a small amount of 3-(trimethylsiloxy)propyl carbamate in a sugar unit of the amylose; and synthesizing into amylose-tri(3,5-dimethylphenylcarbamate) derivatives containing a small amount of 3-(trimethylsiloxy)propyl groups . On that basis, the synthesized amylose derivatives are fully dissolved in tetrahydrofuran, the mixture and tetraethylortho silicate are subjected to crosslinking copolymerization by a sol-gel process, then the product is dispersed and aged in a sodium dodecyl sulfate aqueous solution, and finally, organic and inorganic hybridized silicon spheres with high content of the amylose derivatives are prepared. The surface of the obtained material is subjected to end sealing. The whole synthesis process is simple, mature and easy to control, the yield is high, and therefore, the preparation method can be used for large-scale batch production.

Description

technical field [0001] The invention relates to a preparation method of a chiral microsphere stationary phase material. Background technique [0002] In recent years, with the rapid development of the field of chiral separation and analysis, higher requirements have been put forward for the chiral recognition efficiency and resolution range of chiral stationary phase materials. Chiral stationary phase has become one of the urgent problems to be solved in this field. Among the existing chiral stationary phases, polysaccharide derivative chiral stationary phases are widely used in chromatography due to their good chiral separation performance and wide range of chiral recognition. However, all currently commercially available chiral stationary phases are generally obtained by means of coating or bonding. The content of polysaccharide derivatives is low and the load capacity is limited, which greatly limits the application of stationary phases in the field of large-scale prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/29B01J20/30
CPCB01J20/29
Inventor 沈军杨超李庚
Owner HARBIN ENG UNIV
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