Preparation method of amylose type derivative functional inorganic-silicon-based chiral micro-sphere fixed-phase material

An amylose, derivative technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of low yield, reduced separation efficiency, tailing, etc., achieve high yield, wide source, solve tailing and other problems Effect

Active Publication Date: 2016-08-31
HARBIN ENG UNIV
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  • 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 amylose type derivative functional inorganic-silicon-based chiral micro-sphere fixed-phase material
  • Preparation method of amylose type derivative functional inorganic-silicon-based chiral micro-sphere fixed-phase material
  • Preparation method of amylose type derivative functional inorganic-silicon-based chiral micro-sphere fixed-phase material

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Experimental program
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Effect test

specific Embodiment approach 1

[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 (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

[0026] 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 an amylose type derivative functional inorganic-silicon-based chiral micro-sphere fixed-phase material. The preparation method comprises the following steps: (1) stirring and reflowing dried mirco-crystalline amylose in anhydrous N,N-dimethylacetamide; cooling to a room temperature and then adding lithium chloride; after raising the temperature, adding anhydrous pyridine; after reflowing, adding 3,5-dimethylphenyl isocyanate; continuously stirring and reflowing and adding 3-(trimethoxysilicon) propyl isocyanate and continuously stirring and reflowing; treating with excessive amount of the 3,5-dimethylphenyl isocyanate; (2) dissolving into tetrahydrofuran and adding n-heptanol, ethyl orthosilicate, water and trimethylsilyl chloride; (3) adding into a sodium dodecyl sulfate water solution; (4) adding trimethylsilyl chloride and anhydrous toluene and reacting under a nitrogen gas atmosphere. A synthesis route is clear and feasible, developed in process, simple to operate and easy to realize and has a few of conditions needing to be controlled; 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, which is based on amylose-tris(3,5-dimethylphenylcarbamate) derivative functionalized inorganic silicon-based chiral microspheres Preparation method of 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, at present, all commercial chiral stationary phases are generally obtained by coating or bonding. The content of...

Claims

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Application Information

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IPC IPC(8): B01J20/29B01J20/30
CPCB01J20/29B01J2220/80
Inventor 沈军杨超李庚
Owner HARBIN ENG UNIV
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