Microwave preparation method of cross-linked polymer based on beta-cyclodextrin

A technology of cross-linked polymer and cyclodextrin, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of waste of raw materials, long reaction time, uneven heating, etc., achieve wide application prospects, shorten reaction time, improve Yield effect

Pending Publication Date: 2020-06-16
山西和佳通生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the slow heat transfer rate and uneven heating, the reaction is greatly affected by the temperature gradient, resulting in uneven particle size distribution of cyclodextrin nano-sponge, low product crystallinity, long reaction time, and unsatisfactory actual yield. And with the saturation of the crosslinking reaction, continuing to increase the material will lead to a decrease in its yield, which causes a waste of raw materials to a certain extent, does not conform to the concept of green chemistry, and is also subject to certain restrictions in application

Method used

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  • Microwave preparation method of cross-linked polymer based on beta-cyclodextrin
  • Microwave preparation method of cross-linked polymer based on beta-cyclodextrin
  • Microwave preparation method of cross-linked polymer based on beta-cyclodextrin

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Effect test

Embodiment 1

[0027] A microwave preparation method of a cross-linked polymer based on β-cyclodextrin, comprising the following steps:

[0028] (1) Stir β-cyclodextrin (β-CD, 4.548g, 0.004mol) and solvent N,N-dimethylformamide (DMF, 54g) evenly, add catalyst triethylamine (TEA, 1.7mL, 0.012mol), microwave reaction for 20min at a reaction temperature of 90°C and a microwave power of 800W;

[0029] (2) Add the crosslinking agent diphenyl carbonate (DPC, 6.000g, 0.028mol) to the reaction solution obtained in step (1), and then microwave the reaction for 90min under the condition that the reaction temperature is 90°C and the microwave power is 800W, Cool to room temperature;

[0030] (3) the reaction solution that step (2) is obtained is transferred to the deionized water equivalent to 6 volume times of the reaction solution that step (2) obtains, is 900r / min stirring and dispersing at speed, separates out white gel-like solid, in Centrifuge at 3000r / min for 8min, vacuum filter, wash the soli...

Embodiment 2

[0045] A microwave preparation method of a cross-linked polymer based on β-cyclodextrin, comprising the following steps:

[0046] (1) Stir β-cyclodextrin (4.548g, 0.004mol) and solvent N,N-dimethylformamide (22.74g) evenly, add catalyst triethylamine (0.6mL, 0.004mol), at reaction temperature Microwave reaction for 30 minutes at 80°C and microwave power of 400W;

[0047] (2) Add cross-linking agent diphenyl carbonate (3.424g, 0.016mol) to the reaction solution obtained in step (1), then microwave reaction for 120min at a reaction temperature of 80°C and a microwave power of 400W, and cool to room temperature;

[0048] (3) The reaction solution obtained by step (2) is transferred to deionized water equivalent to 5 volume times of the reaction solution obtained by step (2), stirred and dispersed at 600r / min, and a white gel-like solid is separated out. Centrifuge for 10 min, filter with suction, wash the solid in batches with 40 mL of deionized water to remove unreacted β-CD a...

Embodiment 3

[0052] A microwave preparation method of a cross-linked polymer based on β-cyclodextrin, comprising the following steps:

[0053] (1) Stir β-cyclodextrin (3.405g, 0.003mol) with solvent N,N-dimethylformamide (40.86g), add catalyst triethylamine (2mL, 0.015mol), and the reaction temperature is Microwave reaction for 10 minutes at 100°C and microwave power of 1000W;

[0054] (2) Add the cross-linking agent diphenyl carbonate (6.427g, 0.03mol) to the reaction solution obtained in step (1), then microwave reaction for 30min at a reaction temperature of 100°C and a microwave power of 1000W, and cool to room temperature;

[0055] (3) The reaction solution obtained in step (2) is transferred to deionized water equivalent to 8 volume times of the reaction solution obtained in step (2), stirred and dispersed at 1200r / min, and a white gelatinous solid is separated out at 3500r / min Centrifuge for 6 min, filter with suction, wash the solid in batches with 60 mL of deionized water to rem...

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Abstract

The invention discloses a microwave preparation method of a cross-linked polymer based on beta-cyclodextrin, which comprises the following steps: (1) uniformly stirring beta-cyclodextrin and N, N-dimethylformamide, adding triethylamine, and carrying out microwave reaction; (2) adding a cross-linking agent diphenyl carbonate, carrying out microwave reaction, and cooling to room temperature; (3) transferring the reaction solution into deionized water, performing stirring and dispersing, separating out a white gelatinous solid, carrying out centrifuging and suction filtration, sequentially leaching the solid with deionized water and ethanol, and carrying out vacuum drying to obtain a crude solid product; and (4) crushing the crude solid product obtained in the step (3), carrying out Soxhlet extraction by using absolute ethyl alcohol as a solvent, and drying the obtained solid product to obtain the cross-linked polymer based on beta-cyclodextrin. Compared with a traditional method for preparing NSCD, the method has the advantages that the reaction time is greatly shortened, the yield of the product is remarkably increased, and the crystallinity and the thermal stability of the obtainedproduct are superior to those of a product obtained by a traditional method.

Description

technical field [0001] The invention relates to a microwave preparation method of a cross-linked polymer based on β-CD, which belongs to the field of preparation of functional materials by cross-linked polymers, the field of β-CD synthesis, the field of multifunctional adsorption materials, the field of VOC purification and biomolecular extraction, and the field of water bodies Medium and heavy metal removal field. Background technique [0002] β-cyclodextrin (β-CD) has a cavity structure that is hydrophilic on the outside and hydrophobic on the inside, and can form clathrates with a series of lipophilic organic molecules and biomolecules that match the size of the cavity, but it is not compatible with hydrophilic, metal The inclusion of ions and macromolecular compounds has certain limitations (Trotta E, Zanetti M, Cavalli R, Cyclodextrin-based nanospongesas drug carriers, Beilstein Journal of Organic Chemistry, 2012, 8: 2019-2099). In order to break through this limitatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/24C08J3/28C08L5/16C08K5/109B01J20/24B01J20/30
CPCB01J20/24C08J3/24C08J3/28C08J2305/16C08K5/109
Inventor 张毅民张阳倩乔宗梅闫菊萍
Owner 山西和佳通生物科技有限公司
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