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Preparation method and application of beta-cyclodextrin, graphene oxide and kieselguhr composite

A composite material, cyclodextrin technology, applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc. Mechanical strength, high removal efficiency

Inactive Publication Date: 2016-02-03
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The results show that the adsorption of methylene blue by the adsorbent can reach the adsorption equilibrium after 50 min, and the adsorbent can be easily separated by magnetic field after adsorption, but the adsorption effect is not very ideal

Method used

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Examples

Experimental program
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preparation example Construction

[0029] The preparation steps of graphene oxide include:

[0030] 1g graphite powder and 0.5g NaNO 3 Dissolve in 98% H in an ice-water bath 2 SO 4 solution and keep the temperature below 4°C. After vigorous stirring, 3 g of KMnO was uniformly and slowly added to the solution 4 powder. Control the temperature below 15°C, react for 1h, then raise the temperature to 35°C and stir for 2h. Then, 46 mL of water was slowly added to the flask, and the solution was brown at this time. The temperature was raised to 98°C, and the reaction was carried out for 30 minutes, and the solution turned bright yellow. After that, dilute with 140 mL of distilled water, and then add 10 mL of 30% H 2 o 2 . The mixture was allowed to stand for about 1 h, then the suspension was centrifuged. Fully wash the precipitate with 5% dilute hydrochloric acid and deionized water, adjust the pH value to 5 or 6, until there is no SO in the filtrate 4 2- (with BaCl 2 solution detection), dried in an ov...

Embodiment 1

[0032] (1) In a 200mL beaker, ultrasonically disperse 0.33g graphene oxide in dry 16.5g N,N-dimethylformamide (DMF), centrifuge and transfer the supernatant to a 250mL three-necked flask, add 3.33g Isophorone diisocyanate (IPDI), then dropwise add 0.12g dibutyltin dilaurate (T-12), react in a water bath at 35°C under nitrogen protection for 0.5h, then add 3.33g β - Disperse cyclodextrin in 3.33g N,N-dimethylformamide (DMF) solution, add the above reaction solution, add 0.16g dibutyltin dilaurate (T-12) solution, and react in a water bath at 30°C for 0.5 h, suction filtered, washed, and dried in a vacuum oven at 50°C to obtain β -cyclodextrin-graphene oxide powder, ground for subsequent use;

[0033] (2) In a 200 beaker, dissolve 2.78g of diatomaceous earth in 12mL of an aqueous solution containing 2.78g of NaOH, soak at 55°C for 0.5h, wash with deionized water, dry at 105°C for later use, and take 2.78g β -Cyclodextrin-graphene oxide powder and pretreated diatomaceous earth ...

Embodiment 2

[0036] (1) In a 200mL beaker, ultrasonically disperse 0.45g graphene oxide in dry 31.5g N,N-dimethylformamide (DMF), centrifuge and transfer the supernatant to a 250mL three-necked flask, add 5.28g Isophorone diisocyanate (IPDI), then dropwise added 0.11g dibutyltin dilaurate (T-12), reacted in a water bath at 60°C under nitrogen protection for 1h, and then added 6.75g β - Disperse cyclodextrin in 28.44g N,N-dimethylformamide (DMF) solution, add the above reaction solution, add 0.21g dibutyltin dilaurate (T-12) solution, and react in a water bath at 55°C for 2h , filtered, washed, and dried in a vacuum oven at 50°C to obtain β -cyclodextrin-graphene oxide powder, ground for subsequent use;

[0037] (2) In a 200 beaker, dissolve 7.24g diatomite in 88mL aqueous solution containing 21.02g NaOH, soak at 75°C for 1h, wash with deionized water, dry at 105°C for later use, take 3.62g β -Cyclodextrin-graphene oxide powder and pretreated diatomaceous earth were dissolved in water and...

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Abstract

The invention belongs to the field of macromolecule composite synthesis, and relates to preparation of a beta-cyclodextrin and kieselguhr composite, in particular to a preparation method and application of the beta-cyclodextrin, graphene oxide and kieselguhr composite. The method includes the steps of preparing graphene oxide through an improved Hummers method, preparing beta-cyclodextrin and graphene oxide powder from beta-cyclodextrin and graphene oxide under the effect of isophorone diisocyanate cross-linking agents, mixing beta-cyclodextrin and graphene oxide powder with preprocessed kieselguhr in an ultrasonic mode, and finally obtaining the beta-cyclodextrin, graphene oxide and kieselguhr composite. The material prepared through the method serves as adsorbent, a methylene blue solution serves as an adsorption object, and experimental results show that the composite has a good adsorption effect; when dyes in sewage are processed through the material, the material has the advantages of being easy and convenient to operate and high in adsorption rate and has certain practical value.

Description

technical field [0001] The invention belongs to the field of polymer composite material synthesis and relates to β - preparation of cyclodextrin-diatomaceous earth composite material, especially related to a β - Preparation method and application of cyclodextrin-graphene oxide-diatomite composite material. Background technique [0002] Dyes are substances that can color fibers or other materials, and most of them are organic compounds and are soluble in water. With the rapid development of printing and dyeing, papermaking, plastics, leather and cosmetics processing industries, the demand for dye chemicals is increasing day by day. Dye wastewater contains toxic and harmful groups such as benzene ring group and azo group. This kind of wastewater has deep chroma, high content of organic pollutants, complex components, water quality changes and high biological toxicity, and is difficult to biodegrade, endangering the environment. and human health. my country is recognized as...

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/30C02F1/28C02F101/30
Inventor 邱凤仙闫洁李欣赵浩杨冬亚
Owner JIANGSU UNIV
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