Method for preparing crosslinking cyclodextrin polymer material through microwave assisting

A technology of cross-linking cyclodextrin and polymer materials, which is applied in the fields of chemical instruments and methods, water pollutants, water/sludge/sewage treatment, etc. It can solve the problem that the polymerization reaction of cyclodextrin is not convenient enough and accelerate the modification polymerization reaction , Shorten the reaction time and other issues, to achieve the effect of shortening the reaction time, increasing the reaction temperature, and large specific surface area

Active Publication Date: 2016-09-07
淄博旭尧生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of cyclodextrin polymerization in the prior art that are not convenient enough, provide a microwave-assisted method for preparing cross-linked cyclodextrin polymer materials, optimize the existing preparation process, and speed up the modified polymerization Reaction, to achieve the purpose of shortening the reaction time, increasing the reaction speed, increasing the yield, and reducing the use of organic solvents and waste emissions, to achieve green chemical synthesis

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] This example provides a method for preparing a crosslinked cyclodextrin polymer material by using microwave-assisted modification of cyclodextrin by diisocyanate, and the specific steps are as follows:

[0023] ready with nitrogen (N 2 ) tube, condenser tube, stirrer and thermometer as the reaction vessel, the flask is placed in the microwave generator, and N 2 , After the air in the bottle was purged, 15mL of dimethyl sulfoxide solvent was added, and 0.02g of composite catalyst (5:1 dibutyltin dilaurate and triethylenediamine) was added dropwise. Set the microwave power to 1000W and the microwave frequency to 2450MHz; add 4.09g of β-CD while stirring, add 4.5g of HDI in dimethyl sulfoxide solution dropwise at a rate of 2.5mL / min, microwave radiation 1min, the reaction temperature is 20°C, the purpose is to make the cross-linking reaction complete. Finally, after adding 10 mL of terminator and stirring mechanically for 4 h, the reaction product was washed with a large...

Embodiment 2

[0025] Microwave-assisted preparation of cross-linked cyclodextrin polymeric materials:

[0026] Prepare a four-necked flask with a nitrogen tube, a condenser, a stirrer and a thermometer, place the flask in a microwave generator, and inject N into the flask before the test. 2 , After the air in the bottle was purged, 20mL of dimethyl sulfoxide solvent was added, and 0.04g of composite catalyst (8:1 dibutyltin dilaurate and tributylamine) was added dropwise. Set the microwave power to 700W and the microwave frequency to 2450MHz; add 3.69g of β-CD while stirring, add 5.69g of TDI in dimethyl sulfoxide solution at 4mL / min, microwave radiation for 3min, and mechanically stir the reaction 8h, the reaction temperature is 50°C, the purpose is to make the cross-linking reaction complete. Finally, 15 mL of terminator was added, and the reaction product was washed with a large amount of water (hot water was used to remove β-CD), dried in vacuum for 20 hours, and ground into powder for...

Embodiment 3

[0028] Microwave-assisted preparation of cross-linked cyclodextrin polymeric materials:

[0029] Prepare a four-necked flask with a nitrogen tube, a condenser, a stirrer and a thermometer, place the flask in a microwave generator, and inject N into the flask before the test. 2 , After the air in the bottle was purged, 27ml of dimethyl sulfoxide solvent was added, and 0.2g of composite catalyst (8:1 dibutyltin oxide and triethylamine) was added dropwise. Set the microwave power to 500W, and set the microwave frequency to 2450MHz; add 5.69g of γ-CD while stirring, slowly add 5.89g of MDI-soluble dimethyl sulfoxide solution at 5mL / min, and after microwave radiation for 5min, The reaction was mechanically stirred for 6 hours, and the reaction temperature was maintained at 70° C., in order to complete the cross-linking reaction. The reaction temperature is 70°C, the purpose is to make the cross-linking reaction complete. Finally, 15 mL of chloroform was added and ultrasonically i...

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PUM

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Abstract

The invention relates to a method for preparing a crosslinking cyclodextrin polymer material through microwave assisting. The method is used for preparing an adsorbent material for treating organic waste water. The method includes the steps that diisocyanate is added into cyclodextrin, composite catalysts including a tin catalyst and an amine catalyst are added, and under microwave irradiation, cyclodextrin is subjected to a polymerization reaction to prepare a crosslinking cyclodextrin polymer; used microwave power is 50-1100 W, microwave frequency is 2450 MHz, and the microwave irradiation time is 0-12 min; the prepared crosslinking cyclodextrin polymer material has the advantages of a regular pore structure and a large specific surface area. The polymerization reaction is carried out under the microwave irradiation condition, compared with a reaction without the microwave irradiation condition, on one hand, reaction time is shortened, and on the other hand, the synthesized polymer material has the larger specific surface area and the regular pore structure, the capacity for adsorbing organic pollutant in the organic waste water is improved, and meanwhile the reaction yield is increased.

Description

technical field [0001] The invention relates to the technical field of material synthesis, in particular to a method for microwave-assisted modification of cyclodextrin, and the prepared cross-linked cyclodextrin polymer material can be used as an organic wastewater treatment agent. Background technique [0002] Cyclodextrin (CD), which has a huge cavity structure, generally refers to the starch formed under the action of cyclodextrin glycosyltransferase (Cyclomaltodextrin Glucanotrnsferase, CDTase), composed of more than six glucose units Cyclic oligosaccharides. The most common are α-cyclodextrin (α-CD), β-cyclodextrin (β-CD) and γ-cyclodextrin (γ-CD), which are composed of 6, 7 or 8 glucosyl units, respectively Linked by α-1,4-glucosidic bonds, the molecular shape is a slightly conical ring with a closed cylindrical structure. The outside is a hydrophilic surface, and the inside is a chiral hydrophobic surface with a certain size. lumen. The most notable feature of cyc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/28C08J3/24C08B37/16C02F1/58C02F101/30C02F101/34
CPCC02F1/58C02F2101/30C02F2101/322C02F2101/345C08B37/0012C08J3/24C08J3/28C08J2305/16
Inventor 周玉青李强魏强王小艳许宁李玉龙
Owner 淄博旭尧生物科技有限公司
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