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Preparation method of organic-inorganic hybrid cyclodextrin chiral separation porous monolithic material

A chiral separation, monolithic material technology, applied in other chemical processes, chemical instruments and methods, etc., can solve the problems of limited chiral separation ability, limited dose of chiral selection, poor mechanical properties, etc.

Inactive Publication Date: 2012-10-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mechanical properties of this type of monolithic material are not good, and it can only allow electroosmotic flow to pass through, but the mobile phase cannot pass through. Therefore, its application is mainly limited to electrochromatography.
Inorganic monolithic materials have the characteristics of good mechanical properties and strong tolerance to organic solvents, but they need to be further modified to introduce chiral selectors [Document 4.Chen, Z.L.; Ozawa, H.; Uchiyama, K. ; Hobo, T.Electrophoresis 2003,24,2550.], the amount of chiral selector introduced by this post-column modification method is limited, so that its chiral resolution ability is limited
In addition, it requires more time and manpower, and also affects the reproducibility

Method used

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  • Preparation method of organic-inorganic hybrid cyclodextrin chiral separation porous monolithic material
  • Preparation method of organic-inorganic hybrid cyclodextrin chiral separation porous monolithic material
  • Preparation method of organic-inorganic hybrid cyclodextrin chiral separation porous monolithic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Add 5 mg cetyltrimethylammonium bromide to 60 μL DMF, 190 μL MeOH, 62 μL H 2 O, magnetically stirred at room temperature to dissolve it;

[0027] 2. Slowly add 150 μL VTMS and 125 μL TMOS to the above solution, and hydrolyze in an ice bath for about 1 hour to obtain a uniform and transparent hydrolyzate;

[0028] 3. Combine 20mg mono (6 A -N-allylamino-6 A -deoxy)-β-CD, 50 μL of 10 μM ammonia solution and 1 mg of azobisisobutyronitrile (AIBN) were added to the above hydrolyzate, and sonicated for 3-20 minutes to make it evenly mixed and remove oxygen;

[0029] 4. Use a syringe to introduce the pre-polymerization solution obtained in 3 into a capillary tube with an inner diameter of 75 μm that has been treated with acid and alkali. Seal the remaining pre-polymerization solution in the centrifuge tube with parafilm.

[0030] 5. Put the capillary and centrifuge tube in 4 in a water bath at a temperature of 37°C, and react for 12 hours. At this time, the pre-polymeri...

Embodiment 2

[0034] 1. Add 5 mg cetyltrimethylammonium bromide to 60 μL DMF, 190 μL MeOH, 62 μL H 2 O, magnetically stirred at room temperature to dissolve it;

[0035] 2. Slowly add 150 μL VTMS and 125 μL TMOS to the above solution, and hydrolyze in an ice bath for about 1 hour to obtain a uniform and transparent hydrolyzate;

[0036] 3. Combine 30mg mono (6 A -N-allylamino-6 A-deoxy)-perphenylcarbamoylatedβ-CD, 50 μL of 10 μM ammonia solution and 2 mg of AIBN were added to the above hydrolyzate, and ultrasonically treated for 3-20 minutes to make it evenly mixed and remove oxygen;

[0037] 4. Use a syringe to introduce the pre-polymerization solution obtained in 3 into a capillary tube with an inner diameter of 75 μm that has been treated with acid and alkali. Seal the remaining pre-polymerization solution in the centrifuge tube with parafilm.

[0038] 5. Put the capillary and centrifuge tube in 4 in a water bath at 40°C, and react for 12 hours. At this time, the pre-polymerization s...

Embodiment 3

[0042] 1. Add 5 mg cetyltrimethylammonium bromide to 60 μL DMF, 190 μL MeOH, 62 μL H 2 O, magnetically stirred at room temperature to dissolve it;

[0043] 2. Slowly add 150 μL ATMS and 125 μL TMOS to the above solution, and hydrolyze in an ice bath for about 1 hour to obtain a uniform and transparent hydrolyzate;

[0044] 3. Combine 60mg mono (6 A -N-allylamino-6 A -deoxy)-per(p-chlorophenylcarbamo-ylated)β-CD, 50 μL of 10 μM ammonia solution and 3 mg of AIBN were added to the above hydrolyzate, and ultrasonically treated for 3-20 minutes to make it evenly mixed and remove oxygen;

[0045] 4. Use a syringe to introduce the pre-polymerization solution obtained in 3 into a capillary tube with an inner diameter of 75 μm that has been treated with acid and alkali. Seal the remaining pre-polymerization solution in the centrifuge tube with parafilm.

[0046] 5. Place the capillary and centrifuge tube in 4 in a water bath at 45°C, and react for 12 hours. At this time, the pre-po...

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Abstract

The invention relates to a preparation method of an organic-inorganic hybrid cyclodextrin chiral separation porous monolithic material. The preparation method comprises the following steps that an alkenylsilane coupling agent and an alkoxysilane coupling agent are mixed and are subjected to prehydrolysis; and the hydrolysate is added with alkenyl-containing cyclodextrin or a derivative of the alkenyl-containing cyclodextrin and an organic polymerization reaction initiator so that the alkenylsilane coupling agent and the alkoxysilane coupling agent undergo a polycondensation reaction in situ and the derivative of the alkenyl-containing cyclodextrin and the alkenylsilane coupling agent undergo a radical polymerization reaction in situ, and thus the organic-inorganic hybrid cyclodextrin chiral separation porous monolithic material with specific cyclodextrin derivative groups is obtained. The preparation method provided by the invention has simple processes, allows mild reaction conditions, can adopts different alkenyl-containing cyclodextrin derivatives according to different requirements, and realizes preparation of the organic-inorganic hybrid cyclodextrin chiral separation porous monolithic material.

Description

technical field [0001] The invention relates to the preparation of a novel organic-inorganic hybrid cyclodextrin chiral separation porous monolithic material. Specifically, after mixing the alkenyl silane coupling agent and the alkoxy silane coupling agent, add alkenyl-containing cyclodextrin or cyclodextrin derivatives and organic polymerization initiators and corresponding porogens to make the silane The polycondensation reaction between coupling agents and the free radical polymerization reaction between alkenyl cyclodextrin or alkenyl cyclodextrin derivatives and alkenyl silane coupling agent are carried out in situ to prepare cyclodextrin or specific cyclodextrin derivatives Porous, organic-inorganic hybrid chiral separation monoliths. Background technique [0002] At present, porous monolithic materials have been widely used in liquid chromatography and electrochromatography due to their simple preparation, diverse functions and good permeability. According to the ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16C08G77/42C08J9/28B01J20/29B01J20/30
Inventor 邹汉法张振宾吴仁安
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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