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Preparation method and application of modified cyclodextrin polymer hydrogel

A cyclodextrin polymer, hydrogel technology, applied in the directions of gel preparation, alkali metal compounds, chemical instruments and methods, etc., can solve the problems of small application range and low efficiency, and achieve convenient operation, wide application range, The effect of wide application prospects

Active Publication Date: 2018-07-13
ZHEJIANG FORESTRY UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems that most of the existing hydrogels can only deal with a single pollutant, the efficiency is low, and the application range is small, the present invention proposes a preparation method and application of a modified cyclodextrin polymer hydrogel, which can efficiently and simultaneously Adsorbs two types of pollutants, phenol and heavy metal ions, with a wide range of applications and high adsorption efficiency

Method used

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  • Preparation method and application of modified cyclodextrin polymer hydrogel
  • Preparation method and application of modified cyclodextrin polymer hydrogel
  • Preparation method and application of modified cyclodextrin polymer hydrogel

Examples

Experimental program
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Embodiment 1

[0025] (1) Mix 8g (equivalent to 0.007mol) of β-cyclodextrin with 250mL of 0.45mol / L sodium hydroxide solution, stir and react in a water bath at 3°C ​​for 5h, and add 1.1g (0.005mol) of p-toluenesulfonyl chloride every 1h, Add a total of 0.025 mol. After the reaction is completed, filter under reduced pressure, adjust the pH of the filtrate to 7.0 with 10% hydrochloric acid solution, crystallize at 3°C ​​for 10 hours, filter under reduced pressure, recrystallize with deionized water, and dry under vacuum at 50°C to obtain the intermediate p-toluenesulfonate Acyl-β-cyclodextrin, infrared spectrum as shown in figure 1 shown.

[0026] (2) Mix 4g of p-toluenesulfonyl-β-cyclodextrin, 4.4g of thiourea, and 200mL of 95% ethanol aqueous solution, reflux at 70°C for 24 hours, add 150mL of 20% sodium hydroxide solution, reflux at 50°C for 5h, and 10% hydrochloric acid Adjust the pH of the filtrate to 2.0, recrystallize with deionized water, and then dry it in vacuum at 50°C to obtain ...

Embodiment 2

[0029] (1) Mix 8g (equivalent to 0.007mol) of β-cyclodextrin with 250mL of 0.6mol / L sodium hydroxide solution, stir and react in a water bath at 0°C for 5h, and add 2.2g (0.01mol) of p-toluenesulfonyl chloride every 1h, A total of 0.040 mol was added, after the reaction was completed, suction filtration under reduced pressure, 10% hydrochloric acid solution adjusted the pH of the filtrate to 6.0, crystallization at 0°C for 12 hours, suction filtration under reduced pressure, recrystallization with deionized water, and vacuum drying at 40°C to obtain the intermediate p-toluenesulfonate Acyl-β-cyclodextrin, infrared spectrum as shown in figure 1 shown.

[0030] (2) Mix 4g p-toluenesulfonyl-β-cyclodextrin, 4g thiourea, and 200mL 90% ethanol aqueous solution, reflux reaction at 65°C for 36h, add 150mL15% sodium hydroxide solution, reflux reaction at 50°C for 4h, 10% hydrochloric acid solution to adjust the pH of the filtrate to 3.0, recrystallize with deionized water, and then dr...

Embodiment 3

[0033] (1) Mix 8g (equivalent to 0.007mol), β-cyclodextrin and 250mL 0.8mol / L sodium hydroxide solution, stir in a water bath at 5°C for 3 hours, and add 2.2g (0.01mol) p-toluenesulfonyl chloride every 1h , add a total of 0.03mol, vacuum filtration after the reaction, 10% hydrochloric acid solution to adjust the pH of the filtrate to 8.0, crystallization at 5 ° C for 8 hours, vacuum filtration under reduced pressure, recrystallization with deionized water and vacuum drying at 45 ° C to obtain the intermediate p-toluene Sulfonyl-B-cyclodextrin, infrared spectrum as shown in figure 1 shown.

[0034] (2) Mix 4g of p-toluenesulfonyl-β-cyclodextrin, 8g of thiourea, and 200mL of 80% ethanol aqueous solution, reflux at 60°C for 48 hours, add 150mL of 10% sodium hydroxide solution, and reflux at 60°C for 3h, 10% Adjust the pH of the filtrate to 3.0 with hydrochloric acid solution, recrystallize with deionized water, and then dry it in vacuum at 40°C to obtain a mercapto-grafted β-cyc...

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Abstract

The invention relates to the technical field of sewage treatment, provides a preparation method and application of cyclodextrin polymer hydrogel, and aims at solving the problems that the conventionalhydrogel is capable of treating single pollutants, and is low in efficiency and small in application range. The preparation method is characterized in that beta-cyclodextrin is used as the raw material and is subjected to selective sulfonylation through toluene sulfochloride to obtain toluenesulfonyl-beta-cyclodextrin; then the toluenesulfonyl-beta-cyclodextrin is subjected to thiourea substituting to obtain hydrosulphonyl grafted beta-cyclodextrin; finally, the hydrosulphonyl grafted beta-cyclodextrin is processed according to a suspension emulsion polymerizing method to obtain the novel two-functional polymer hydrogel. The hydrogel prepared according to the method is applicable to a complex sewage system integrating phenol and heavy metal ions. The hydrogel is capable of efficiently synchronously adsorbing two pollutants including phenol and the heavy metal ions, and is wide in application range and high in adsorption efficiency.

Description

technical field [0001] The invention relates to the technical field of sewage treatment, in particular to a preparation method and application of a modified cyclodextrin polymer hydrogel for synchronously identifying and adsorbing molecular / ion pollutants in a sewage system. Background technique [0002] With the development of industrialization and urbanization, the massive discharge of industrial and domestic wastewater has caused serious water pollution, directly threatening the growth of animals and plants as well as human health and living environment. Sewage treatment has received unprecedented attention. Organic pollutants and heavy metal ions are the most important components in sewage. Currently, there are membrane separation methods, adsorption methods, chemical methods, biological methods, etc. to treat such pollutants. Most of the above methods are only for a single pollutant, and the cost is high Inefficient and time-consuming. Therefore, efficient sewage treat...

Claims

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Application Information

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IPC IPC(8): C08J3/075C08J3/24C08B37/16C08F251/00C08F222/38C08L5/16C08K5/29C08K5/1515B01J20/24B01J20/28C02F1/28B01J13/00C02F101/20
CPCB01J13/0065B01J20/24C02F1/286C08B37/0012C08F251/00C08J3/075C08J3/24B01J20/28047C02F2101/20C02F2101/345B01J2220/4806B01J2220/4825B01J2220/4812C08J2305/16C08K5/1515C08K5/29C08F222/385
Inventor 郭明朱寅帆卢闻君孙立苹
Owner ZHEJIANG FORESTRY UNIVERSITY
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